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《化学试剂》2021年第5期中英文摘要

发布时间: 2021-05-07 15:39:01   试剂信息网


气相色谱-质谱联用技术在食药检测中的应用与发展

邓高琼,陈亨业,刘瑞,付海燕*

(中南民族大学 药学院,湖北 武汉  430074

 

摘要:气相色谱-质谱联用(Gas chromatography-mass spectrometry, GC-MS)是一种结合色谱高分离能力和质谱高鉴别能力的在线分离、定性和定量检测技术,适用于挥发性成分的分析。近年来,随着样品前处理技术及配套仪器的不断发展,GC-MS技术的分离性能越来越好、检测灵敏度越来越高,使其被广泛应用于食药领域中的成分分析、品质分析、掺假鉴别和有害物检测等方面。本文综述了目前常用的样品前处理技术以及近5GC-MS在食药检测相关领域的应用,旨在阐明GC-MS在食药检测领域中的重要意义,明确其性能特点,总结其优缺点,并对其未来发展进行展望。

关键词:气质联用;前处理技术;成分分析;品质分析;有害物检测

中图分类号:O657.7    文献标识码:A      文章编号:0258-3283(2021)—

 

Application and Development of Gas Chromatography-Mass Spectrometry Technology in Food and Chinese Herbal Medicine Testing DENG Gao-Qiong, CHEN Heng-Ye, LIU Rui, FU Hai-Yan*(School of Pharmaceutical Sciences, South-Central University for Nationalities, Wuhan 430074, China), Huaxue Shiji, 2021, 43(5),

AbstractGas chromatography-mass spectrometry (GC-MS) is an online separation, qualitative and quantitative detection technology that combines high chromatographic separation capabilities and high discrimination capabilities of mass spectrometry. It is suitable for the analysis of volatile components. Due to its good separation performance and high detection sensitivity, this technology is widely used in ingredient analysis, quality analysis, adulteration identification and pesticide residue detection in the food and medicine field. In this paper, the application of GC-MS in food and drug detection related fields in the past five years was reviewed, aiming to clarify the significance of GC-MS in food and drug detection field, clarify its performance characteristics, summarize its advantages and disadvantages, and forecast its future development.

Key wordsGC-MS; pretreatment technology; food and Chinese herbal medicine testing; component analysis; quality analysis; pesticide residue

引用本文邓高琼, 陈亨业, 刘瑞, . 气相色谱-质谱联用技术在食药检测中的应用与发展[J]. 化学试剂, 2021, 43(5): 555-562.


 

气相色谱-嗅辨仪/质谱联用法对龙井茶中差异标志物的高通量筛查

范尧1,陈云吟1,李爱兰1,张磊1,周春松1,2,付海燕1,佘远斌*1

(1.浙江工业大学 化学工程学院,浙江 杭州  3100322.宜兴国际环保城科技发展有限公司,江苏 宜兴  214200)

 

摘要:龙井茶为中国十大名茶之首,其特征成分决定了其品质差异。因此,研究龙井茶成分群并寻找差异标志物对其质控起着重要的作用。利用气相色谱-嗅辩仪(GC-O) 和气相色谱-质谱 (GC-MS) 结合移动窗口偏最小二乘判别分析 (MWPLSDA) 方法,确定了可以区分不同产地和等级龙井茶的5种差异标志物。通过比较不同色谱变量范围获得的偏最小二乘模式识别(PLSDA)结果,各差异标志物的代表性排序为戊醛> (Z) -3-己烯-1-醇和3-烯烃>苯甲醇> 2-乙基-1-己醇。此外,当选择戊醛对应色谱变量区间时,可实现对六种龙井的100%区分。

关键词:气相色谱-嗅辩仪;气相色谱-质谱;龙井茶;移动窗口偏最小二乘判别分析;差异标志物

中图分类号:O69      文献标识码:A      文章编号:0258-32832021--

 

High-throughput screening of differential markers in Longjing teas through GC-O/GC-MS FAN Yao1, CHEN Yun-yin1, LI Ailan1, ZHANG Lei1, ZHOU Chun-song1,2, FU Hai-yan1, SHE Yuan-bin*1 (1. State Key Laboratory Breeding Base of Green Chemistry-Synthesis Technology, College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310032, China2. International Environmental Protection City Technology Co. Ltd., Yixing 214200, China)

AbstractLongjing tea ranks first in China’s top ten famous tea, which quality is determined by its characteristic components. Therefore, studying the constituents of Longjing tea and finding out its differential markers play important role for its quality control. In this study, gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS) combined with the moving window partial least squares discriminant analysis (MWPLSDA) model were used to determined five differential markers for recognition of Longjing teas with various geographical origins and grades based on. In addition, by comparing the recognition results obtained by choosing different ranges of variables, the representative ranking of these five differential markers was sorted as valeraldehyde > (Z)-3-hexen-1-ol and 3-carene > benzyl alcohol > 2-ethyl-1-hexanol. Most importantly, the accuracy of PLSDA for the six different Longjing samples was as high as 100% by selecting the chromatographic variable interval corresponding to valeraldehyde.

Key wordsGC-O; GC-MS; Longjing teas; MWPLSDA; differential markers

引用本文:范尧, 陈云吟, 李爱兰, . 气相色谱-嗅辨仪/质谱联用法对龙井茶中差异标志物的高通量筛查[J]. 化学试剂, 2021, 43(5): 563-569.

 

 

气质联用自动化解析方法分析花生成熟期的挥发与半挥发性有机物

于永杰*1,赵娟娟1,郭晓萌1,王允2,孙涛1,韩璐1,李淑芳2

(1. 宁夏医科大学  药学院,宁夏回族自治区 银川  7500042. 河南省农业科学院农业质量标准与检测技术研究所,河南 郑州 450002)

 

摘要:花生进入饱果成熟期之后,籽粒成熟过程中代谢物变化影响着收获花生的品质和营养价值。本文通过化学计量学领域最新发展的气质联用自动化解析方法结合非靶向代谢组学技术,对饱果成熟期的花生在收获前一个月、收获前半个月和收获时等三个不同采收时间的花生籽粒中挥发、半挥发性成分进行了分析。通过直接对仪器采集原始信号进行解析鉴定出数十种化合物。在化学成分解析的基础上,利用偏最小二乘判别分析方法实现了不同采收时间样本的判别分析。

关键词:气质联用;代谢组学;化学计量学;花生籽粒;数据自动分析

中图分类号:O657      文献标识码:A      文章编号:0258-32832021--

 

Automatic data analysis methodology for gas chromatography-mass spectrometry to analyze volatility and semi-volatility compounds during the maturation stage of peanut seed YU Yong-Jie*1, ZHAO Juan-Juan1, GUO Xiao-Meng1, WANG Yun2, SUN Tao 1, HAN Lu1, LI Shu-Fang2 (1. College of  Pharmacy, Ningxia Medical University, Yinchuan 750004, China; 2. Institute of Quality Standard and Testing Technology for Agro-products, Henan Academy of Agricultural Science, Zhengzhou 450002), Huaxue Shiji, 2021, 43(5),

AbstractThe metabolite changes during the maturation process of peanut seed play an important role for the quality and nutritive value of harvested peanuts. The present work proposes a methodology for analyzing volatility and semi-volatility compounds in peanut seeds during the maturation stage, which is accomplished by introducing a recently proposed automatic chemometric gas chromatography-mass spectrometry (GC-MS) data analysis methodology in combination with untargeted metabolomics. Samples from three ripening stages were collected, i.e., a month before harvest period, a half month before the harvest period, and the harvest period. The raw GC-MS data files were analyzed and tens of metabolites were identified. Finally, principal component analysis was used for discriminating samples from different periods.

Key wordsGC-MS; metabolomics; Chemometrics; Peanut seed; Automatic data analysis methodology

引用本文于永杰, 赵娟娟, 郭晓萌, . 气质联用自动化解析方法分析花生成熟期的挥发与半挥发性有机物[J]. 化学试剂, 2021, 43(5):570-575.

 

 

吹扫捕集-气质联用结合化学计量学用于不同产地和品牌浓香型白酒鉴别

李爱兰1,乔文君1,汪兴财1,范尧1,贾俊杰1,2,王松涛2,周春松3,付海燕1,佘远斌*1

(1.   浙江工业大学 化学工程学院,浙江 杭州 3100322. 泸州老窖有限公司,四川 泸州 646000 3.宜兴国际环保城科技发展有限公司,江苏 宜兴  214200

摘要:不同地域生态环境的差异和生产厂家酿造工艺的差异,使得不同产地和品牌白酒具有不同的挥发性成分。本研究通过吹扫捕集-气质联用技术对浓香型白酒的产地和品牌进行快速鉴别。基于浓香型白酒的挥发性成分差异性,通过偏最小二乘判别分析(OPLS-DA)可对其产地和品牌进行准确区分,且预测能力指数Q2Y值均大于0.5,具备较好的预测能力。通过变量投影重要性(VIP)分析及挥发性成分含量计算,分别筛选出辛酸乙酯、乙酸异丙烯酯等8种与产地密切相关以及异戊酸乙酯、二糠基醚、2-甲基戊烷等6种与品牌密切相关的挥发性成分。这些产地和品牌标志性成分的确定可对白酒的快速鉴别奠定良好的理论基础。

关键词:浓香型白酒;化学计量学;GC-MS;产地鉴别;品牌鉴别

中图分类号:O657.7      文献标识码:A      文章编号:0258-3283(2021)--

 

Purge and trap-GC/MS combined with chemometrics for identification of strong aroma baijiu from different origins and brands LI Ai-lan1, QIAO Wen-jun1, WANG Xing-cai1, FAN Yao1, JIA Jun-jie1,2, WANG Song-tao2, ZHOU Chun-song3, FU Hai-yan1, SHE Yuan-bin* 1(1. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310032, China2. Luzhou Laojiao Co. Ltd., Luzhou 646000, China3. International Environmental Protection City Technology Limited Company (IEPCT), Yixing 214200, China), Huaxue Shiji, 2021, 43(5),

Abstract: Due to the differences of ecological environment in different regions and the differences in the brewing technology of manufacturers, different regions and brands of baijiu have different volatile components. In this study, the origin and brand of strong aroma baijiu were quickly identified by the technology of purge and trap-GC/MS. Based on the difference involatile components of strong aroma baijiu, the origin and brandof strong aroma baijiu could be accurately distinguished through the orthogonal partial least squares discriminant analysis (OPLS-DA), and the predictive ability index Q2Y value was greater than 0.5, which indicated that it had a good predictive ability.Through the variable projection importance (VIP) analysis, 8 kinds of volatile components, such as ethyl caprylate, isopropenyl acetate, etc., which were closely related to the origin, and 6 kinds of volatile components, such as ethyl isovalerate, difurfuryl ether, 2-methylpentaneetc, etc., were selected, which were closely related to the brand.The identification of these origins and brand iconic ingredients could lay a good theoretical foundation for the rapid identification of baijiu.

Keywords: strong aroma baijiu; chemometrics; GC-MS; identification of origin; identification of brand

引用本文李爱兰,乔文君,汪兴财,等.吹扫捕集-气质联用结合化学计量学用于不同产地和品牌浓香型白酒鉴别[J].化学试剂, 2021, 43(5): 576-583.

 

 

气质联用结合化学计量学对中国白菊特征挥发性成分的研究

海城英1,白秀云1,陈亨业1,杨小龙1,杨健2,付海燕*1

(1. 中南民族大学 药学院,湖北 武汉 4300742. 中国中医科学院中药研究所,北京 100700)

 

摘要:为探究不同产地中国白菊的特征挥发性成分,利用吹扫捕集-气相色谱质谱联用技术(Purge-and-trap-gas chromatography-mass spectrometry, P&T-GC-MS)对江苏如东、湖北蒋场、湖北黄潭、河南武涉、北京延庆5个产地的菊花样品的挥发性成分进行检测,利用autoGCMSDataAnal策略及化学计量算法对其特征挥发性成分进行筛选。结果共获得醇、烯、酯、烷烃等多种共有化合物。其中,α-蒎烯、菊油环酮等化合物在如东菊花中含量最高,2,6-二甲基-5,7-辛二烯-2-醇在延庆菊花中含量最高,桉叶油醇在武涉县菊花中含量最高,Β-倍半水芹烯、β-石竹烯等在蒋场镇菊花中含量最高。另外,基于上述特征化合物的判别模型可对菊花的产地进行精准判别,准确率可达98%以上。本研究筛选的特征挥发性成分可为菊花的产地溯源提供一定的理论基础。

关键词:菊花;气相色谱-质谱联用;化学计量学;挥发性成分;风味物质

中图分类号:R917       文献标识码:A       文章编号:0258-32832021--

 

Study on characteristic volatile components of Chinese White Chrysanthemum by GC-MS combined with Chemometrics HAI Cheng-ying1, BAI Xiu-yun1, CHEN Heng-ye1, YANG Xiao-long1, YANG Jian2, FU Hai-yan*1 (1. School of Pharmacy, South-Central University for Nationalities, Wuhan 430074, China; 2. Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China), Huaxue Shiji, 2021, 43(5),

Abstract To explore the characteristic volatile components of Chinese White Chrysanthemum (Chrysanthemum morifolium Ramat.) from different producing areas, Purge-and-trap-gas (P&T-GC-MS) chromatography-mass spectrometry (P&T-GC-MS) was used to test the volatile components of C. morifolium samples from five origins which in Rudong, Jiangchang, Huangtan, Wushe and Yanqing. Then autoGCMSDataAnal strategy and chemometrics were used to identify the volatile components in the chrysanthemum samples. The result showed that chrysanthemum contains many compounds such as alcohols, alkenes, esters, and alkanes. Among them, α-pinene, chrysanthenone and other compounds have the highest content in Rudong samples; 2,6-dimethyl-5,7-octadien-2-ol has the highest content in Yanqing samples; eucalyptol has the highest content in Wushe samples, b-sesquiphellandrene and β-caryophyllene have the highest content in Jiangchang samples. Besides, the discriminant model based on the above-mentioned characteristic compounds can accurately discriminate the origin of C. morifolium samples with an accuracy rate of over 98%. The characteristic volatile components selected in this study can provide a theoretical basis for the traceability of the origin of Chinese White Chrysanthemum.

Key wordsChrysanthemum; P&T-GC-MS; Chemometrics; Volatile components; Flavor substances

引用本文海城英,白秀云, 陈亨业, 等. 气质联用结合化学计量学对中国白菊特征挥发性成分的研究[J]. 化学试剂, 2021, 43(5): 584-589.

 

制备条件对针铁矿-生物炭复合物汞砷吸附性能的影响

迪力夏提·阿不力孜

(乌鲁木齐职业大学 经济贸易学院,新疆 乌鲁木齐  830001

摘要在不同原料配比、酸碱度、陈化时间和陈化温度下,通过Fe(NO3)3·9H2O沉淀合成了不同的针铁矿-生物炭复合物(GBC),对未修正生物炭及其复合产物进行了扫描电镜、红外光谱和X-射线衍射表征,最后选用吸附效果较好的针铁矿-生物炭复合物进行汞砷吸附试验。结果表明,原生物炭样品为黑色颗粒物,经针铁矿复合后变为褐黑色状态并且表面覆盖一层柱状或针状物。FTIR光谱在31251465803782640 cm-1处出现几个与针铁矿有关的吸收峰。XRD图谱中出现与针铁矿特征峰相符的`几个衍射峰,其中不同原料配比、不同酸碱度制备的复合物XRD图谱相差较大,而不同陈化温度和陈化时间下制备的复合物XRD图谱无明显差异。按照金属吸附实验结果,汞和砷吸附效率最高的针铁矿-生物炭复合物的制备条件可确定为:m(生物炭)m(Fe(NO3)3·9H2O) = 16pH7、陈化温度40 ℃、陈化时间40 h

关键词生物炭;针铁矿;汞吸附;砷吸附;制备条件

中图分类号TQ424.1+9    文献标识码A   文章编号0258-32832021

 

Effect of Preparation Conditions of Goethite Biochar Composite on Mercury and Arsenic Adsorption Properties DILIXIATI Abulizi (College of Economics and Trade Urumqi Vocational University, Urumqi 830001, China), Huaxue Shiji, 2021, 43(5),

Abstract: Goethite biochar composite (GBC) were synthesized by precipitation of Fe(NO3)3·9H2O under different raw material ratio, pH, aging time and temperature. The original biochar and its composite products were confirmed by scanning electron microscope, infrared spectrum and X-ray diffraction. Finally, the goethite biochar composite with better adsorption effect was selected for mercury and arsenic adsorption test. The original biochar samples are black particles, which become brown black after being compounded by goethite and covered with a layer of columnar or needle like substances. In FTIR spectra, there are several absorption peaks related to goethite at 3125, 1465, 803, 782 and 640 cm-1. There are several diffraction peaks which are consistent with the characteristic peaks of goethite. The XRD patterns of the composites prepared by different raw material ratio and different pH value have great difference, but the XRD patterns of the composites prepared under different aging temperature and aging time have no obvious difference. Based on the results of metal adsorption experiment, the preparation conditions of goethite biochar composite with the best adsorption performance on mercury and arsenic can be determined as follows: the mass ratio of biochar to Fe(NO3)3·9H2O is 1:6, pH > 7, aging temperature is 40, aging time is 40 h.

Key words: biochar; goethite; Hg(II) removal; As (III) removal; synthesis conditions

引用本文:迪力夏提•阿不力孜. 制备条件对针铁矿-生物炭复合物汞砷吸附性能的影响[J]. 化学试剂, 2021, 43(5):590-597.

 

 

备方法对Fe-Mn-Ox催化剂的NH3-SCR反应性能影响

任婉婷,邢赟,张庭基,刘威,张学军*

(沈阳化工大学 环境与安全工程学院,辽宁 沈阳  110142

 

摘要:NOx是目前主要大气环境污染物之一,去除NOx是大气净化领域研究的热点,其中Fe-Mn-Ox催化剂去除NOx的效率较高。对Fe-Mn-Ox催化剂进行了一系列研究,采用共沉淀(CP)、水热(HT)、溶胶凝胶(SG)方法分别制备了该催化剂,对这3种催化剂的NH3-SCR性能进行了探究。制备方法会对催化剂的活性产生较多影响,影响因素有MnFe物种的存在状态、催化剂的可还原性、催化剂的孔容、催化剂的平均孔径、催化剂的表面酸性等。结果证明,水热法制备的Fe-Mn-Ox催化剂催化活性最佳。

关键词:氮氧化物;选择性催化还原;制备方法;催化剂

中国分类号:X511     文献标识码:    文章编号:0258-32832021--

 

Effect of Preparation Methods on Performance of Fe-Mn-Ox Catalyst for NH3-SCR Reaction Ren Wan-ting, Xing Yun, Zhang Ting-ji, Liu Wei, Zhang Xue-jun*( School of Environmental and Safety Engineering, Shenyang University of Chemical Technology, Shenyang, 110142), Huaxue Shiji, 2021, 43(5),

AbstractNOx is one of the major atmospheric environmental pollutants, and NOx removal is a hotspot in the field of atmospheric purification. Among them, Fe-Mn-Ox catalyst has a high efficiency in NOx removal. Fe-Mn-Ox catalysts were prepared by co precipitation (CP), hydrothermal method (HT) and sol-gel (SG) respectively. The NH3-SCR properties of the three catalysts were investigated. The difference of preparation methods will have a lot of influence on the activity. There are many influencing factors, such as the existing state of Mn and Fe species, the reducibility of the catalyst, the pore volume of the catalyst, the average pore size of the catalyst, the surface acidity of the catalyst, etc. All these factors have a series of effects on SCR activity. The Fe-Mn-Ox catalyst prepared by hydrothermal method has the best catalytic activity.

Key wordsnitrogen oxide; selective catalytic reduction; preparation method; catalyst

引用本文:任婉婷,邢赟,张庭基,等.制备方法对Fe-Mn-Ox催化剂的NH3-SCR反应性能影响[J].化学试剂,2021, 435):598-603.

 

 

基于网络药理学探究银杏叶提取物治疗脑血管痉挛的作用机制

罗祥敏1a,雷芳1a,彭俊超1a,都国栋1b,王鲁2,何珺*2

1.贵州大学 a. 药学院,b.化学与化工学院,贵州贵阳 5500252.贵州省生化工程中心,贵州贵阳550025

 

摘要:基于网络药理学方法预测银杏叶提取物治疗脑血管痉挛的潜在靶点及信号通路,阐述其作用机制。利用TCMSP平台筛选银杏叶中生物利用度(OB30%和类药性(DL0.18的活性成分,GeneCardsSwiss Target prediction数据库检索脑血管痉挛疾病相关蛋白靶点和活性成分的相关靶点,并用Venny平台获取活性成分与脑血管痉挛疾病之间的共有靶点,STRING数据库构建靶蛋白之间的相互作用网络图(PPI),进行GO生物功能模块分析、KEGG通路富集分析,并采用Cytoscape软件构建可视化的“活性成分-潜在靶点”网络图。从银杏叶中筛选出27个活性成分,脑血管疾病和活性成分共有靶点82个,银杏叶提取物治疗脑血管痉挛疾病涉及到EDNRAAPOBEGFREGFEDN1等多个靶点,以及HIF-1信号通路、肿瘤坏死因子信号通路、类风湿性关节炎等相关通路。银杏叶提取物具有治疗脑血管痉挛疾病的功效可能是由多个活性成分作用于多个相关靶点,通过调节多个通路的共同结果。

关键词:网络药理学;银杏叶提取物;潜在靶点;信号通路;作用机制

中图分类号:R285.5 文献标识码:A

 

To explore the mechanism of ginkgo biloba extract in the treatment of cerebral vasospasm based on the network pharmacologyLUO Xiang-min1a, LEI Fang1a, PENG Jun-chao1a, DU Guo-dong1b, WANG Lu2, HE Jun*2 (1.College of Pharmacy, Guizhou University, Guiyang 550025, China; 2. Research Center of Biochemistry Engineering of Guizhou Province, Guiyang 550025,China ; 3.College of Chemistry and Chemical Engineering, GuizhouUniversity,Guiyang 550025, China )

ABSTRACT: To predict the potential target and signal pathway of ginkgo biloba extract in the treatment of cerebral vasospasm based on the network pharmacology method, and to elaborate the mechanism of action.Compounds whose bioavailability (OB) ≥30% and drug-likeness  (DL) ≥0.18 in ginkgo biloba leaves were screened by TCMSP platform. Related targets of active components and related protein targets of cerebral vasospasm disease were retrieved using GeneCards and Swiss Target Prediction databases, and the common targets of active components and cerebral vasospasm disease were extracted using Venny platform. STRING database was used to construct interaction network diagram (PPI) between target proteins, GO biological function module analysis and KEGG pathway enrichment analysis were carried out, and Cytoscape software was used to build visual "compound-potential target" network diagram. 27 Active ingredients were selected from ginkgo biloba leaves, with a total of 82 targets for compounds and cerebral vasospsam diseases. The treatment of cerebral vasospasm withginkgobiloba extracts involve multiple targets such as EDNRA, APOB, EGFR, EGF, EDN1, and related pathways such as HiF-1 signaling pathway, Tumor necrosis factor signaling pathwayand rheumatoid arthritis. The efficacy of ginkgo bilobaextract in the treatment of cerebral vasospasm may be the result of multiple active components acting on multiple related targets and regulating multiple pathways.

Key Words: Network pharmacology; Ginkgo biloba extract; Potential targets; Signal path; Mechanism of action

引用本文:罗祥敏,雷芳,彭俊超,等.基于网络药理学探究银杏叶提取物治疗脑血管痉挛的作用机制[J].化学试剂,2021,435604-609.

 

 

焙烧复原法制备山梨酸和苯甲酸插层水滑石及其缓释性能研究

李木子1,郑秀君*1,任德财2

1黑龙江东方学院 食品与环境工程学部,黑龙江 哈尔滨  1500662黑龙江工程学院 材料与化学工程学院,黑龙江 哈尔滨  150050

 

摘要:焙烧复原法无需有机溶剂,制备流程比较简单,条件容易控制。以水滑石(LDH)为载体,通过焙烧复原法分别将山梨酸(SA)和苯甲酸(BA)插入其层间,制备了SA-LDHBA-LDH插层材料。采用傅里叶变换红外光谱(FTIR)、X-射线衍射(XRD)、热重-差热分析(TG-DSC)和扫描电镜(SEM)对其结构和热稳定性进行表征,并研究在不同pH缓冲体系中的缓释性能和机理。结果表明,SABA阴离子成功的插入到LDH层间,分散效果得到了明显改善。SA-LDH表现出良好的缓释性能,在pH 4.43.4的缓冲溶液中120 min后达到释放平衡,释放量分别为431.34389.38 mg/gBA-LDH存在突释现象,缓释性能不佳,释放时间为30 min时达到平衡,在pH 4.43.4的缓冲溶液中释放量为353.22304.17 mg/gSABA的释放过程符合准二级动力学方程。焙烧复原法制备的SA-LDH材料具有良好的缓释性能,在防腐保鲜类食品包装材料中的应用具有重要意义。

关键词:水滑石;山梨酸;苯甲酸;缓释;载体

中图分类号:O 614     文献标识码:A     文章编号:0258-32832021--

 

Sorbic Acid and Benzoic Acid Intercalated Hydrotalcite via Calcine-Recovering Method: Preparation and Release Performances LI Mu-zi1, REN De-cai*2, ZHENG Xiu-jun*1 (1.Department of Food and Environmental Engineering, Heilongjiang East University, Harbin 150066, China; 2.School of Materials and Chemical Engineering, Heilongjiang Institute of Technology, Harbin 150050, China)

Abstract: The calcine-recovering method does not require organic solvents, the preparation process is relatively simple and the conditions are easy to control. The intercalated materials of SA-LDH and BA-LDH were obtained by intercalation of SA and BA into the sheets of hydrotalcites (LDH) via calcine-recovering method. The structure and thermal stability of intercalated materials were confirmed by FTIR, X-ray diffractionXRD, TG-DSC and SEM. The release performances of SA-LDH and BA-LDH materials were investigated in different pH buffer systems. Both SA and BA anions were successfully intercalated in the interlayer and the dispersion was improved obviously. SA-LDH had a good drug controlled release performance, the release amounts of SA-LDH were 431.34 mg-1 and 389.38 mg-1 in buffer solutions at pH 4.4 and 3.4 after 120 min, respectively. BA-LDH had a sudden release phenomenon and poor release performance, the release amounts of BA-LDH were 353.22 and 304.17 mg-1 in buffer solutions at pH 4.4 and 3.4 after 30 min, respectively. The SA and BA release kinetic process can be fitted well by pseudo-second-order. By using calcine-recovering method, SA-LDH materials with good release performances were successfully prepared, which is of great significance for the application of LDH in anti-corrosion and fresh-keeping food packaging materials.

Key words: hydrotalcites; sorbic acid; benzoic acid; release; carrier

引用本文:李木子,郑秀君,任德财. 焙烧复原法制备山梨酸和苯甲酸插层水滑石及其缓释性能研究[J].化学试剂,2021435610-616.

 

木质素磺酸季铵盐两性表面活性剂的合成和性能

赵小红*,蒙燕霞

(贺州学院 材料与化学工程学院,广西 贺州  542899

 

摘要针对木质素利用率低造成环境污染与资源浪费问题,以木质素磺酸钠为原料制备木质素磺酸季铵盐两性表面活性剂,对合成工艺和产品性能进行系统研究,以期为木质素的变废为宝提供参考。结果表明,最优的合成条件为:n(木质素磺酸钠)n(中间体) = 11.1、反应时间2.5 h、反应温度50 ℃pH 12,影响反应的主要因素是pH值,其次是物质的量比,反应时间和温度,产物活性物质含量为51.6%w)。红外光谱和紫外光谱分析表明反应后在酚羟基中引入了烃基。产物具有较低的表面张力、较强的分散力和发泡性能,在酸性和碱性溶液中溶解性良好、亲水性较强、乳化性能一般,在洗涤剂等方面具有应用潜力。

关键词:木质素;季胺盐;两性表面活性剂;制备;性能

中图分类号TQ423  文献标识码A     文章编号0258-32832021--

 

Synthesis and Properties of a Lignin Sulfonate Quaternary Ammonium Salt Amphoteric Surfactant ZHAO Xiao-hong*, MENG Yan-xia (College of Materials and Chemical Engineering, Hezhou University, Hezhou 542899,China), Huaxue Shiji, 2021, 43(5),

AbstractIn the light of low utilization of lignin which causes environmental pollution and waste of resources, a lignin sulfonate quaternary ammonium salt amphoteric surfactant was synthesized from sodium lignosulfonate. The synthesis process and product performance were systematically investigated so as to provide reference for the waste reuse of lignin. The optimal synthesis conditions were as follows: n(sodium lignosulfonate)n(intermediate) = 1:1.1, reaction time 2.5 h, reaction temperature 50 ℃, pH 12. The factors affecting the reaction have the decreasing order of pH, molar ratio, reaction time and temperature. The content of active substance was 51.6% (w) under the optimal synthesis conditions. FTIR and UV analyses of product showed that hydrocarbon radical was introduced into the phenolic hydroxyl. The product has low surface tension, strong dispersion and foaming properties, good solubility in acidic and alkaline solutions, strong hydrophilicity, but normal emulsifying properties. It has potential applications in detergents and other fields.

Key words: lignin; quaternary ammonium salt; amphoteric surfactant; preparation; properties

引用本文:赵小红,蒙燕霞. 木质素磺酸季铵盐两性表面活性剂的合成和性能[J]. 化学试剂, 2021, 43(5):617-621

 

 

抗菌水凝胶在生物医学领域的研究进展~

张浩然,王士凡*,朱文友,庄文昌,董黎明,堵锡华

(徐州工程学院 材料与化学工程学院,江苏 徐州 221018)

 

摘要:细菌感染是阻碍伤口愈合的重要因素之一,同时也是生物医学领域面临的一个重要问题。目前的抗菌水凝胶有着高抗菌活性、生物相容性以及可注射性等性能,并且其物理化学性质与生物组织相似,使得越来越多新型的抗菌水凝胶材料被用于治疗细菌感染。综述了近几年抗菌水凝胶的研究进展,归纳总结了几种不同类型的抗菌水凝胶的制备方法,抗菌活性和生物相容性等。重点阐述了抗菌水凝胶在伤口敷料、药物负载和传递以及组织工程等生物医学领域中的应用前景。

关键词:水凝胶;抗菌活性;生物相容性;生物医学

中图分类号:O063      文献标识码:A      文章编号:0258-32832021-

 

Progress of Antibacterial Hydrogel in Field of Biomedicine ZHANG Hao-ran, WANG Shi-fan*, ZHU Wen-you , ZHUANG Wen-chang, DONG Li-ming, DU Xi-hua (School of Materials and Chemical Engineering, Xuzhou Institute of Technology, Xuzhou 221018, China), Huaxue Shiji, 2021, 43(5),

AbstractBacterial infection is one of the important factors hindering wound healing, and it is also an important problem in biomedical field. The current antibacterial hydrogels have high antibacterial activity, biocompatibility and inject ability, and their physical and chemical properties are similar to those of biological tissues, making more and more new antibacterial hydrogel materials used to treat bacterial infections. The research progress of antibacterial hydrogels in recent years was reviewed, and summarizes the preparation methods, antibacterial activity and biocompatibility of several kinds of antibacterial hydrogels. Furthermore, the application prospect of antibacterial hydrogels in wound dressings, drug loading and delivery, tissue engineering and other biomedical fields are emphasized.

Key Wordshydrogel; antibacterial activity; biocompatibility; biomedicine

引用本文:张浩然,王士凡,朱文友,等.抗菌水凝胶在生物医学领域的研究进展[J].化学试剂,2021, 435):622-631.

 

 

微流控技术在食品安全快速检测中的应用

朱婧旸1,2董旭华1,2沈佳彬1,2,刘海泉1,2,赵勇*1,2朱永恒*1,2

1. 上海海洋大学 食品学院,上海 2013062. 上海市水产品加工与保鲜工程技术研究中心  上海  201306

 

摘要:在当今的全球一体化食品供应链中,确保食品质量和安全至关重要。微流控技术(Microfluidic Technology)作为近年来发展迅速的全新微量分析技术,其具有的连续化、微型化、智能化等独特优势推动了现场快速检测技术的发展,使样本消耗微量化以及多参数同步检测等检测需求成为可能。目前,微流控技术已在临床诊断、食品安全、环境科学、生物检测等领域得到了广泛应用。主要介绍了微流控芯片技术的研究进展,概括了近年来其在食品安全快速检测方面的应用,针对其不同的检测原理、结构及性能进行了讨论,并对其应用前景和发展趋势进行了展望。

关键词:微流控技术;食品质量安全;快速检测

中图分类号:TS201.6       文献标识码:A      文章编号0258-32832021--

 

Application of microfluidic technology in food safety rapid detection Zhu Jing-yang1,2, Dong Xu-hua1,2, Shen Jia-bin1,2, Liu Hai-quan1,2, Zhao Yong*1,2, Zhu Yongheng*1,2 (1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China; 2. Shanghai Engineering Research Center of Aquatic Product Processing & Preservation, Shanghai 201306, China), Huaxue Shiji, 2021, 43(5),

Abstract: Assuring the safety and quality of food is vital in today’s worldwide integrated food supply chain. In this context, microfluidic is a new technology that has developed rapidly in recent years. Its unique advantages of continuity, miniaturization, and intelligence have promoted the development of on-site rapid detection technology, and it also makes it possible to minimize sample consumption and multi-parameter synchronous detection. At present, microfluidic technology has been widely used in clinical diagnosis, food safety, environmental science, biological detection and other fields. This review mainly introduced the recent progress of microfluidic technology, summarized its application in food safety rapid testing, and discussed its different testing principles, structure and performance, finally put forward its application prospects and development trends, in order to provide a good guide for food safety monitoring.

Key words: microfluidic technology; food quality and safety; rapid detection

引用本文:朱婧旸, 董旭华, 沈佳彬, . 微流控技术在食品安全快速检测中的应用[J]. 化学试剂, 2021, 43(5):632-639.

 

 

人工智能在物肝脏毒性预测中的应用

杜潇楠1,周慧宇1,王玉成*1,李雪梅*2

1. 中国医学科学院 北京协和医学院医药生物技术研究所,北京 1000502. 国家药品监督管理局药品审评中心,北京 100022

摘要:药物性肝损伤(Drug-induced liver injury, DILI)是导致药物终止临床试验和退出市场的主要原因,由于评价候选药物潜在毒性的动物模型和体外细胞模型物种间的一致性较差、无法模拟人体内复杂的环境等原因导致准确度较低。随着组合化学和高通量筛选技术的发展产生了大量数据,并推动了人工智能和学习算法的进步,越来越多的人工智能应用于药物性肝损伤研究,提高了预测药物肝脏毒性的准确性。为了比较不同的建模算法在药物肝脏毒性预测中的优劣并为今后的研究提供一定的参考,对近十年使用人工智能针对肝脏毒性开发的QSAR模型进行了综述。

关键词:药物性肝损伤;药物毒性;人工智能;机器学习;定量构效关系(QSAR

中图分类号:R9      文献标识码:A      文章编号:0258-32832021--

 

Application of Artificial Intelligence in the Prediction of Drug Hepatotoxicity DU Xiao-nan1, ZHOU Hui-yu1, WANG Yu-cheng*1, LI Xue-mei*2 ( 1. Institute of Medical Biotechnology, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100050; 2.Center For Drug Evaluation, NMPA), Huaxue Shiji, 2021, 43(1),

Abstract: Drug-induced liver injury (DILI) is the main reason for drug candidates to suspend clinical trials and withdrawal from the market. Animal models and in vitro cell models used in evaluating the potential toxicity of drug candidates are in accurate due to poor interspecies consistency and inability to simulate complex environments in vivo. With the development of combinatorial chemistry and high-throughput screening techniques, the generation of large amounts of data promotes the advancement of artificial intelligence and learning algorithms. More and more machine artificial intelligence has been applied to the study of drug-induced liver injury, which improves the accuracy of predicting drug liver toxicity. In order to dicuss the advantages and disadvantages of different modeling algorithms in the prediction and provide some references for future researchwe summarized the QSAR model for hepatotoxicity using machine learning in the past ten years.

Key words: drug-induced liver injury; drug toxicity; artificial intelligence; machine learning; QSAR

引用本文杜潇楠,周慧宇,王玉成, . 人工智能在药物肝脏毒性预测中的应用[J]. 化学试剂, 2021, 43(5):640-648.

 

 

制定化学试剂储存标准原则和内容的探究

宋金链,郭培*,刘岩,张键鑫

(天津市康科德科技有限公司,天津301701

 

摘要:化学试剂品种多、数量小、应用范围广,目前存在法规空白与现实管理的脱节,有必要制定化学试剂储存的标准。制定该标准应当坚持科学量化管理、融合行业经验、借鉴国内国际标准规范、科技赋能、应急优先和问题导向等原则。该标准应当建立符合化学试剂储存的有限数量包装,包装要符合跌落和堆码等安全性能要求,按照危险性细化分级、分级管理、分类施策,推进化学试剂储存管理的信息化、数字化和智能化应用,制定应急管理要求,确定储存管理规范。制定本标准,意在破解化学试剂行业发展的瓶颈,建立化学试剂规范化管理体系,破解现实使用的困境和监管的难题,推动化学试剂依法监管、理性监管、科学监管水平。

关键词:化学试剂;储存;标准;原则;内容;依法监管;理性监管;科学监管

中图分类号:O6-1     文献标识码:A     文章编号:0258-3283(2021)

 

Principles and Contents of Constituting Chemical Reagents Storage Standards SONG Jin-lian, GUO Pei*, LIU Yan, ZHANG Jian-xin (Tianjin Concord Technology Co., Ltd., Tianjin 301701, China), Huaxue Shiji, 43(5),

Abstract: Chemical reagents have a large number of varieties, small packaging specifications, high quality requirements, and a wide range of applications. To address the gap between regulations and practical management of chemical reagents, it is necessary to make standards for chemical reagents storage. The formulation of this standard should adhere to the principles of scientific quantitative management, consider integration of industry experience, reference domestic and international standards and norms, empower technological, prioritize emergency and be problem orientated. The standard should be established in accordance with the limitation on packing quantity for chemical reagents and in compliance with requirement of safety performances such as drop and stacking. In accordance with the detailed classification, hierarchical management, and classification of policies, the new standard should promote the information, digitalization and intelligent application of chemical reagent storage management, formulate emergency management requirements, and determine storage management standards. The formulation of this standard is intended to break the bottleneck of the development of chemical reagents industry by establishing a standardized management system for chemical reagents, closing the gap of practical use and regulations, and promoting the legal, rational and scientific supervision of chemical reagents.

Key words: chemical reagents; storage; standards; principles; content; supervision of law; rational supervision; scientific supervision

引用本文:宋金链, 郭培, 刘岩, . 制定化学试剂储存标准原则和内容的探究[J]. 化学试剂, 2021, 43(5):649-654.

 

 

丹皮药材-饮片-配方颗粒中5种重金属的含量及溶出特性研究

李宗金,喻格,张玲*

安徽中医药大学 药学院,安徽 合肥  230012

 

摘要:通过原子吸收光谱法、原子荧光光谱法分别测定牡丹皮药材、饮片、配方颗粒及不同提取物中铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、铜(Cu5种重金属的含量。结果表明,所有牡丹皮样品中5种重金属含量均在《中国药典》和《药用植物及制剂进出口绿色行业标准》规定的标准限下,且5种重金属的含量高低顺序为Cu>As>Pb>Cd>Hg。牡丹皮药材中PbCu含量高于饮片及配方颗粒中的含量,而CdHgAs 3种元素含量则低于饮片或配方颗粒中的含量。3种提取物中检测出的重金属含量高低为As>Cd>Hg,均未检测出PbCu,牡丹皮水提液、醇提液中As的溶出率最高,分别为86.67%70.00%,其次是Hg在水提液中的溶出率为60.91%。该方法简便快速、灵敏度高、干扰较少、结果可靠。该研究结果可为进一步控制牡丹皮药材中重金属含量提供参考,为保证牡丹皮药材品质及用药安全性评价提供依据。

关键词:丹皮;重金属;溶出特性;原子吸收光谱法;原子荧光光谱法

中图分类号:R284     文献标识码:A         文章编号:0258-32832021--

 

Five Heavy Metals Concentration in Moutan Cortex and Dissolution Characteristics LI Zong-jin, YU Ge, ZHANG Ling* (School of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China), Huaxue Shiji, 2021, 43(5),

Abstract: The contents of five heavy metals: leadPb, cadmiumCd, mercuryHg, arsenicAs and copper Cuin the medicinal materials, decoction pieces, formula granules and different extracts of Moutan Cortex were determined by atomic absorption spectrometry and atomic fluorescence spectrometry. The contents of the five heavy metals in all the samples of Moutan Cortex were within the standard limits specified in  Chinese Pharmacopoeia and Green Industry Standard for import and export of medicinal plants and preparations, and the contents of five heavy metals followed the following order: Cu>As>Pb>Cd>Hg. The contents of Pb and Cu in the medicinal materials of Moutan Cortex were higher than that in the decoction pieces and formula granules, while the contents of Cd, Hg and As were lower than that in the decoction pieces or formula granules. The contents of heavy metals detected in the three extracts decreased in the order: As>Cd>Hg, and Pb and Cu were not detected. The dissolution rates of As in the water extract and alcohol extract of Moutan Cortex were the highest, 86.67% and 70.00% respectively. The dissolution rate of Hg in the water extract was 60.91%. This method is simple, fast, sensitive, less interference, and reliable. The results provide a reference for further controlling the content of heavy metals in the medicinal materials of Moutan Cortex, and provide a research basis for ensuring the quality of Moutan Cortex and the safety evaluation of drugs.

Key words: Moutan Cortex; heavy metals; dissolution characteristics; atomic absorption spectrometry; atomic fluorescence spectrometry

引用本文李宗金,喻格,张玲. 牡丹皮药材-饮片-配方颗粒中5种重金属的含量及溶出特性研究[J]. 化学试剂,2021435655-659.

 

 

Box-Behnken设计优化浊点萃取-原子荧光法分析环境水样中无机砷形态

郝晓棠,姜勋,刘炜婷,谢美仪,刘甜恬,王梅*

(广东药科大学公共卫生学院,广东广州 510310)

 

摘要:建立浊点萃取-原子荧光光谱法分析水样中无机砷形态的新方法。以派洛宁B为络合剂、Triton X-114为萃取剂,对As(III)进行萃取。选择溶液pH值、派洛宁B用量、Triton X-114用量以及水浴温度为自变量,荧光值为响应值,采用单因素分析和Box-Behnken设计方法,研究各自变量及其交互作用对荧光值的影响。结果表明,各因素对荧光值的影响程度依次为:pH派洛宁B用量Triton X-114浓度,且Triton X-114pH、水浴温度存在交互作用。在最优条件下,As(III)0.44.0mg/L浓度范围内与荧光强度有良好的线性关系,方法检出限为0.025mg/L,相对标准偏差为1.37%n=6),对于50mL样品溶液,富集倍数为9.4倍。该方法成功用于水样中无机砷形态分析,加标回收率为96.7%105%,获得了满意的结果。

关键词:浊点萃取;砷;形态分析;Box-Behnken设计;响应面法

中图分类号:O657.3X703文献标识码:A      文章编号:0258-32832021

 

Cloud Point Extraction-Atomic Fluorescence Spectrometry for Determination of InorganicArsenic Species in Water Samples with Box-Behnken Design HAO Xiao-tang, JIANG Xun, LIU Wei-ting, XIE Mei-yi, LIU Tian-tian, WANG Mei*(School of Public Health, Guangdong Pharmaceutical University, Guangzhou 510310, China), Huaxue Shiji, 2021, 43(5),

Abstract: A novel cloud point extraction approach was developed for the preconcentration and determination of inorganic arsenic species in water samples prior to HG-AFS. As(III) wascomplexed with Pyronine B and then quantitatively extracted by the non-ionic surfactant (Triton X-114). Fourexperimental factors including Pyronin B dose, pH, Triton X-114 dose and epuilibrium temperature for CPE were selected as the independent variables. The individual and interactive effects of these factors on the fluorescence intensity were investigated using a single factor experiment and a Box-Behnken design. The influence of each factor on fluorescence value was as follows: pHPyronin B doseTriton X-114 concentration. Interactions between Triton X-114 and pH,Triton X-114 and temperature affected the response value. Under the optimized conditions, a good linearity was obtained in the concentration range of 0.44.0mg/L for As(III) with the relative standard deviation of 1.37%(n=6). The limit of detection was 0.025mg/Land the enrichment factor was 9.4 for a 50mL sample. The proposed method was successfully applied for inorganic arsenic speciation analysis in water samples, with satisfactory recoveries of 96.7%105%.

Key words:cloud point extraction; arsenic; speciation analysis;Box-Behnken design; response surface methodology

引用本文:郝晓棠, 姜勋, 刘炜婷, . Box-Behnken设计优化浊点萃取-原子荧光法分析环境水样中无机砷形态[J]. 化学试剂, 2021, 43(5):660-665.

 

 

QuEChERS快速前处理法测定人参、西洋参及其制品中杀线威等7种农药

王金子1王佳慧2付瑶2胡婷婷2黄炜婷2张鑫2张勋*2

1.国家药品监督管理局高级研修学院,北京1000002. 长春海关技术中心,吉林长春 130062

 

摘要:建立了检测人参、西洋参及其制品中杀线威、敌百虫、多菌灵、吡虫清、硫双威、丙硫克百威、除虫菊酯7种农药的液相色谱-串联质谱检测分析方法。样品经乙腈超声提取,QuEChERS法净化,滤膜过滤后用液相色谱-串联质谱法进行定性和定量分析。结果表明:7种农药的浓度在0.010.2mg/L范围内呈现良好的线性关系(相关系数R20.998),7种农药的检出限为0.01 mg/kg。分别选取生晒白参、西洋参、人参蜜片、西洋参蜜片样品,在0.010.020.2mg/kg3个浓度水平下进行加标回收试验,7种农药的加标回收率在80.0%103.1%之间,相对标准偏差为4.86%8.09%( n = 6)。该前处理方法简便快捷、对目标物定性定量准确,适用于大量人参及人参制品的快速准确测定。

关键词:人参;西洋参;QuEChERS;农药;液相色谱-串联质谱法

中图分类号:O657.63      文献标识码:A      文章编号:0258-32832021--

 

Determination of SevenPesticide Residues in Ginseng and American Ginseng and Their Products using QuEChERS Rapid Pretreatment Method WANG Jin-zi1, WANG Jia-hui2, FU Yao2, HU Ting-ting2, HUANG Wei-ting2, ZHANG Xin2, ZHANG Xun*2(1.Advanced Research Institute of State Drug Administration, Beijing 100000, China; 2.Changchun Customs Technology Center, Changchun 130062, China), Huaxue Shiji, 2021, 43(5),

Abstract: To establish a method for the simultaneous determination of 7 pesticide residues in Ginseng and Ginseng products by liquid chromatography-tandem masss pectrometry (LC-MS/MS). After extracted by acetonitrile, the filtrate was purified by QuEChERS and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS).The calibration curves for 7 analysts showed correlation coefficients better than 0.998, and the quantification limits were 0.01 mg/kg. The average recoveries of 7 pesticides at the spiked levels of 0.010.020.2mg/kg ranged from80.0%103.1% with RSDs of 4.86%8.09%( n = 6). It has been proved that this new method with many advantages such as simplicity in operation, economical and rapid clean-up procedure. The method is suitable for rapid and accurate determination of Ginseng and American ginseng and their products.

Key words: ginseng; american ginseng; QuEChERS; pesticides; LC-MS /MS

引用本文:王金子,王佳慧,付瑶,等. QuEChERS快速前处理法测定人参、西洋参及其制品中杀线威等7种农药[J]. 化学试剂, 2021, 43(5):666-670.

 

 

电感耦合等离子体质谱的钡中毒检验方法研究

李想,夏鑫鑫,朱昱*

(中国刑事警察学院,辽宁 沈阳  110854

 

摘要:建立了碰撞反应池-电感耦合等离子体质谱分析测定中毒案件中胃内容和血样钡元素含量的研究方法。通过优化消解液体系、消解时间和消解温度,确定样品前处理的最优消解条件。用碰撞反应池技术降低电感耦合等离子质谱分析中多原子分子造成的干扰。研究结果表明,钡的检出限为0.40 ng/g,回收率在94.80%105.75%之间,说明所建立的方法具有灵敏度高、准确度高和线性范围宽等优势,适用于胃内容和血中钡含量的检验,可确定中毒或者死亡原因、中毒来源和摄入途径。

关键词:碰撞反应池;电感耦合等离子体质谱;胃内容;血

中图分类号:O655.1+1    文献标识码A     文章编号0258-32832021

 

Detection of Barium Poisoning by Inductively Coupled Plasma Mass Spectrometry LI Xiang, XIA Xin-xin, ZHU Yu* (Criminal Investigation Police University of China, Shenyang 110854, China), Huaxue Shiji, 2021, 43(5),

Abstract: The method of inductively coupled plasma mass spectrometry (ICP-MS) with the kinetic energy discrimination model (KED) was established for the determination of barium concentration in stomach and blood samples of poisoning cases. By optimizing the digestion liquid system, digestion time and digestion temperature, the optimal digestion conditions for sample pretreatment were determined. In the method, KED was used to eliminate interference from the polyatomic molecules. The limit of detection for barium was 0.40 ng/g. The recovery rates ranged from 94.80%105.75%. The developed methods had the advantages of high sensitivity, high accuracy and wide linear range. It was suitable for examining barium concentration of stomach and blood samples and was used to determine the cause of poisoning or death, source of poisoning and route of ingestion.

Key words: kinetic energy discrimination model (KED); Inductively Coupled Plasma-Mass Spectrometry (ICP-MS); gastric content; blood

引用本文:李想,夏鑫鑫,朱昱. 电感耦合等离子体质谱的钡中毒检验方法研究[J]. 化学试剂,2021435671-675.

 

 

纸上色层分离—硫酸铁铵滴定法测定钛铝铌合金中钛的含量

李甜,田新,胡梦桥,陈雄飞*,陈映纯,王雪菲,张力久

(国标(北京)检验认证有限公司,北京 100088

 

摘要:滴定钛铝铌合金中钛元素时,由于铌易水解形成沉淀,往往干扰滴定终点的判断和结果的准确度。实验采用纸上色层分离-硫酸铁铵滴定法测定钛铝铌合金中钛的含量。以硝酸-氢氟酸溶解试样,采用纸上色层分离技术将铌与钛分离,在酸性条件下,用铝片将Ti4+还原为Ti3+,以硫氰酸钾作为指示剂,用硫酸铁铵标准溶液滴定至砖红色为终点。按照上述实验方法测定2个实际样品中钛含量,结果的相对标准偏差RSD分别为0.27% 0.23%n=11),加标回收率为98.5%~102.4%。方法有良好的精密度和准确度,可用于钛铝铌合金中钛含量的分析。

关键词:色层分离;硫酸铁铵滴定法;钛铝铌;钛

中图分类号:O655.23      文献标识码A    文章编号0258-3283(2021)--

 

Determination of Titanium in Titanium-aluminum-niobium Alloys by Separation of Paper Chromatography—Ammonium Ferric Sulfate Titration Method LI Tian, HUMeng-qia, CHEN  Xiong-fei, CHEN Ying-chun, Wang Xue-Fei, Tian Xin, Zhang Li-jiu (Guobiao(Beijing) Testing & Certification Co., Ltd., Beijing 100088, China), Huaxue Shiji, 2021, 43(5),

AbstractThe content of titanium in titanium-aluminum-niobium alloy was determined by ammonium ferric sulfate titration. The sample was dissolved with nitric acid and hydrofluoric acid and the niobium and titanium were separated by using a paper color separation technique. Under acidic conditions, Ti4+is reduced to Ti3+ by aluminum flakes, a saturated sodium bicarbonate solution was used as a protective solution to prevent Ti3+ oxidation. The potassium thiocyanate is used as an indicator and the standard solution of ammonium ferric sulfate is titrated to red as the end point. Based on the consumption of volume of the ammonium ferric sulfate, the titanium content in the sample is obtained. The titanium content in the two samples was determined via the experimental method. The relative standard deviations (RSD, n = 11) of the results were 0.27% and 0.23% with the spiked recoveries were in the range of 98.5%~102.4%. The method can be used for the analysis of titanium content in titanium-aluminum-niobium alloy.

Key wordschromatographic separation; Ammonium ferric sulfate titration; titanium-aluminum-niobium alloys; titanium

引用本文:李甜,田新,胡梦桥,等. 纸上色层分离—硫酸铁铵滴定法测定钛铝铌合金中钛的含量[J].化学试剂,2021435676-679.

 

 

一种新型快速筛查水中多氯联苯的方法

崔君*1,2,3,4,顾华1,3,4,刘慧青5,温晓华1,3,4

1. 国土资源部上海资源环境监督检测中心,上海2000722.上海市地质勘查技术研究院,上海2000723.上海市地质调查研究院,上海2000724.自然资源部地面沉降监测与防治重点实验室,上海 2000725.东华大学化学化工与生物工程学院,上海201620

 

摘要:近年来对于水中持久性有机物的生产和排放的管控日渐增强,但持久性有机物依然是环境健康潜在的危险所在。对于这些持久性化合物的监测和评估不得不依赖昂贵且费时的常规方法。本研究介绍了一种新型的基于荧光检测多氯联苯的快速检测方法,基于苯并a芘(BaP)与多氯联苯(PCB)之间形成的交互作用从而使BaP荧光强度随着PCB的浓度的增大而增强。从而实现不用复杂前处理,即可以通过荧光检测BaP的强度判断PCB的浓度含量等级。为了确定这种交互作用的选择性和基质影响性,对pH,离子强度模拟实际地下水条件也展开了研究。结果表明,这些条件对于PCB/BaP间的作用影响很小,从而增大了将此方法应用于实际检测的可能性。

关键词:多氯联苯;荧光检测;苯并a芘;快速筛查

中图分类号:O656.22O657.39      文献标识码A      文章编号0258-32832021--

 

A Novel Method for Rapid Screening of Polychlorinated Biphenyls in Water CUI Jun*1,2,3,4,GU Hua1,3,4,LIU Hui-qing5,WEN Xiao-hua1,3,4 (1.Shanghai Resources Environment Supervision and Inspection Center, Ministry of Land and Resource, Shanghai200072, China;2. Shanghai Institute of Geological Prospecting Technology, Shanghai200072, China; 3.Shanghai Institute of Geological Survey,Shanghai200072, China;4.Key Laboratory of Land Subsidence Monitoring and Prevention,Ministry of Natural Resources, Shanghai200072, China;5.College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai201620, China), Huaxue Shiji, 2021, 43(5),

Abstract: Although the control of the production and discharge of persistent organic matter in water has increased in recent years, persistent organic matter remains potential danger to human health. Despite obtainedgreat attention, the monitoring and evaluation of these persistent compounds has relied on expensive and time consuming conventional methods. A novel method for the detection of polychlorinated biphenyls based on fluorescence detection was described. The interaction between benzopyrene (BaP) and polychlorinated biphenyls (PCB) enhanced with increased PCB concentration which reflected on BaP fluorescence intensity. Therefore, it is possible to initially determine the concentration level of PCB by detecting the intensity of BaP by fluorescence. In order to determine the selectivity and matrix influence of this interaction, the actual groundwater conditions for pH and ionic strength simulation were also investigated. These conditions had little effect on the interaction between PCB/BaP, which increased the possibility of applying this method to actual detection. The number of chlorine atoms in the PCB has a significant effect on the interaction of PCB/BaP.

Key words: polychlorinated biphenyls (PCB); fluorescence detection;benzopyrene(BaP); rapid screening

引用本文:崔君, 顾华, 刘惠青, . 一种新型快速筛查水中多氯联苯的方法[J]. 化学试剂, 2021, 43(5):680-684.

 

 

水中8种金属元素混合溶液系列标准物质的研制

胡雪静*1季红梅1王以堃2黄成浩1付朝阳1朱培娟1

(1.南京市计量监督检测院,江苏南京 2100492.江苏省计量科学研究院,江苏南京 210023)

 

摘要:采用国家有证纯金属系列标准物质和高纯铁成份分析标准物质制备了水中PbCdCuFeZnCrNiCo 8种金属元素混合溶液系列标准物质,用一级标准物质对其进行比较定值。使用电感耦合等离子体发射光谱法考察其均匀性与稳定性,结果表明所研制的0.5125 mg/L系列标准物质的均匀性和稳定性良好,有效期12个月。分析了该系列标准物质的不确定度来源,评定其相对扩展不确定度为3%k=2)。该系列标准物质浓度呈梯度排列,可直接用于食品检测中标准曲线的绘制,为ICP-OESICP-MS检测中多金属元素分析带来便利。

关键词:混合金属元素标准物质;均匀性检验;稳定性检验;不确定度;食品检测

中图分类号TQ421.3      文献标识码A     文章编号0258-3283(2021)--

 

Development of Standard Substances for Eight Metal Elements Mixed Solution in WaterHUXue-jing*1, JI Hong-mei1, WANG Yi-kun2, HUANG Cheng-hao1, FU Chao-yang1, ZHU Pei-juan1 (1. Nanjing Institute of measurement and testing technology, Nanjing 210049, China; 2.Jiangsu Institute of Metrology, Nanjing 210023, China), Huaxue Shiji, 2021, 43(5),

AbstractA series of reference materials of mixed solution containing Pb, Cd, Cu, Fe, Zn, Cr, Ni and Co were prepared by using national certified pure metal reference materials, and their values were determined by first-class reference materials. The uniformity and stability of them were investigated by inductively coupled plasma emission spectrometry (ICP-AES). The 0.5, 1, 2, 5mg/L series of standard substances had good uniformity and stability and were valid for 12 months. The source of uncertainty of standard substances was analyzed, and the relative extended uncertainty was assessed as 3% (k =2). This series of concentration standard substances are arranged in gradient, which can be directly used to establish standard curve in food detection, which brings convenience for the analysis of polymetallic elements in the ICP-OES and ICP-MS detection.

Key wordsMixed metallic element reference materials; Uniformity test; Stability test; Uncertainty; Food detection

引用本文:胡雪静,季红梅,王以堃,等. 水中八种金属元素混合溶液系列标准物质的研制[J]. 化学试剂,2021435685-691.

 

 

吖啶-苯并咪唑鎓环番化合物在检测H2PO4-中的应用

董智云,韩喜龙,王迎进,席福贵*

(忻州师范学院 化学系,山西 忻州 034000)

 

摘要以一种吖啶-苯并咪唑鎓环番化合物L为荧光传感器,在化合物LV(乙腈):V(水)= 95 : 5溶液中加入H2PO4-后导致荧光发射峰(Em = 426 nm)猝灭,检出限为4.75 × 10-7 mol/LJob曲线显示化合物LH2PO4-离子之间以1 : 1化学计量比结合,结合常数为(6.96 ± 0.44×104 L/mol。在波长为365 nm紫外灯照射下,化合物L发出明显的蓝绿色荧光,而L-H2PO4-络合物呈现较弱的蓝色荧光,可实现固态检测H2PO4-阴离子。DFT计算显示化合物L通过苯并咪唑2HH2PO4-离子之间形成了非常强的离子型氢键。

关键词:吖啶;环番化合物;苯并咪唑鎓;H2PO4-;荧光传感器

中图分类号:O626.1      文献标识码:A      文章编号:0258-3283(2021)--

 

Application of Aridine-Benzimidazolium Cyclophane in the Detection of H2PO4- DONG Zhi-yun, HAN Xi-longWANG Ying-jin, XI Fu-gui*(Department of Chemistry, Xinzhou Teachers UniversityXinzhou, Shanxi, 034000, China)

AbstractAn aridine-benzimidazolium cyclophane L was used as a fluorescent sensor, compound L displayed excellent sensitivity specific toward H2PO4-. The fluorescence emission peak at 426 nm was quenched when H2PO4- was added to the VCH3CN):VH2O= 95 : 5 solution of sensor L and the detection limit was 4.75 × 10-7 mol/L. The 1 : 1 stoichiometry was verified by Job’s plot, and the association constant was obtained to be (6.96±0.44)×104 L/mol. The sensor L emitted obvious blue-green fluorescence by the naked eye under UV lamp irradiation at 365 nm, while the complex of L-H2PO4- exhibited weaker blue fluorescence, which can realize recognition of H2PO4- anions on solid-state. DFT showed that H2PO4- located up the cave of compound L and formed hydrogen bond with the C2H proton of benzimidazoliums.

Key wordsAridine; Cyclophane; Benzimidazolium; H2PO4-; Fluorescent sensor

引用本文董智云,韩喜龙,王迎进,等. 吖啶-苯并咪唑鎓环番化合物在检测H2PO4-中的应用[J]. 化学试剂, 2021, 43(5): 692-697.

 

 

不同取代基的苯甲醛制备相应取代基的乙炔苯

罗磊,王勇*

 (荆楚理工学院 药物合成与优化湖北省重点实验室,湖北 荆门  448000)

 

摘要:通过4步反应获得了12种不同取代基的乙炔基苯,并以良好或优异的产率得到了末端炔烃。即通过不同取代基苯甲醛与丙二酸发生Knoevenagel反应得到了不同取代基的3-苯基丙烯酸;在冰醋酸存在下,将不同取代基的3-苯基丙烯酸分别与液体溴反应,得到相应取代基的23-二溴-3-苯基丙酸;含不同取代基的2-溴乙烯基苯是由相应取代基的23-二溴-3-苯基丙酸在Et3N/DMF中的反应合成;通过化合物不同取代基的2-溴乙烯基苯与氢氧化钾的反应得到所需产物不同的取代基乙炔基苯。 当取代基为溴时,产物具有最佳产率,而当取代基为硝基和叔丁基时,产率低。这表明不同的电子效应对产物的产率有很大的影响。

关键词:炔烃;Knoevenagel反应;取代基;合成;醛

中图分类号:O621.3      文献标识码:A      文章编号:  0258-3283(2021)--

 

Preparation of Different Substituent Ethynylbenzene from its Corresponding Benzaldehyde Luo Lei, WANG Yong* (Hubei Key Laboratory of Drug Synthesis and Optimization, Jingchu University of Technology, Jingmen 444800, China), Huaxue Shiji, 2021, 43(5),

Abstract12 Different substituents of ethynylbenzene were obtained, and terminal alkynes were obtained with good or excellent yield through the following four steps. Different substituents of 3-phenylacrylic acid were given by reaction of different substituents of benzaldehyde with malonic acid by Knoevenagel condensation. Reaction of different substituents of 3-phenylacrylic acid with liquid bromine in the presence of glacial acetic acid afforded 2, 3-dibromo-3-phenyl propanoic acid with corresponding substituents. 2-Bromovinylbenzene with different substituents was synthesized from the reaction of 2,3-dibromo-3-phenylpropionic acid with corresponding substituents in an Et3N/DMF system. Ethynylbenzene with different substituents of the desired product was obtained by reaction of 2-bromovinylbenzene with different substituents with potassium hydroxide. When the substituent is bromine, the product has the best yield, and when the substituent is nitro and tert-butyl, the yield is low. This indicates that different electronic effects have a great effect on the yield of the products.

Key wordsalkyne; Knoevenagel reaction; substituents; synthesized; aldehyde

引用本文:罗磊,王勇.同取代基的苯甲醛制备相应取代基的乙炔苯[J]. 化学试剂,2021, 435698-704.

 

 

分子内还原Heck反应合成7--1-茚满酮

牟芃兴滕大为*

(青岛科技大学化工学院,山东青岛266042)

 

摘要:研究了标题化合物的合成新方法,即以邻溴苯甲酸为原料,经取代反应、氧化还原反应、格氏反应以及分子内还原Heck反应合成了目标化合物。探讨了分子内还原Heck反应中反应溶剂、反应温度、反应时间及催化剂种类等条件对产率的影响。最终确定了以四氢呋喃为溶剂、Pd(dppf)Cl2为催化剂、60℃反应6 h的最佳反应条件,产率可达83%

关键词:7--1-茚满酮;2--6--苯甲酸;氧化反应;分子内还原Heck反应

中图分类号:O625.29文献标识码:A文章编号:

 

Synthesis of 7-Bromo-1-Indanone via an Intramolecular Reductive Heck ReactionMu Peng-xing,TengDa-wei*(College of Chemistry Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)

Abstract: A new synthetic method of the title compound was studied. The target product was synthesized from 2-Bromobenzoic acid by substitution reaction,oxidation-reduction reaction, Grignard Reaction and Intramolecular Reductive Heck Reaction. The effects of reaction solvents,temperature,reaction time and kinds of catalyst in Intramolecular Reductive Heck Reaction were investigated. Finally, the optimum reaction conditions were determined with tetrahydrofuran as the solvent, Pd(dppf)Cl2 as the catalyst and 60℃ for 6 hours, and the yield could reach 83%.

Key words7-bromo-1-indanone;2-bromo-6-iodobenzoic acid;oxidationreaction;Intramolecular Reductive Heck Reaction

引用本文:牟芃兴,滕大为. 分子内还原Heck反应合成7--1-茚满酮[J].化学试剂,2021,435705-709.