核酸检测试剂盒专利技术发展态势研究
屈缨虹*，罗啸，谢楠，王莉，高东辉
（北京三聚阳光知识产权代理有限公司，北京 100080）
摘要：核酸检测试剂盒由于具有检测灵敏度高、特异性强、检测速度快等特点，被广泛应用到医疗诊断、生物医药、食品检测等领域，是目前各国竞相研究的技术热点，更是全球疫情流行状态下的关注焦点。从专利数据出发，通过对核酸检测试剂盒领域相关专利进行检索，以全球/中国专利申请数量分布、主要竞争国家、专利技术来源国和目标国、主要申请人等为分析指标，得出该领域专利技术发展与创新趋势、竞争态势以及研发热点规律，为我国在该领域的科技创新提供参考。
关键词：核酸检测；试剂盒；专利分析；发展态势
中图分类号：G306 文献标识码：A 文章编号：0258-3283（2020）
Research on Patent Technology Development Trend Analysis of Nucleic Acid Detection Kit QU Ying-hong*, LUO Xiao, XIE Nan, WANG Li, GAO Dong-hui (SUNSHINE INTELLECTUAL PROPERTY INTERNATIONAL CO., LTD, Beijing 100080, China), Huaxue Shiji, 2020, 42（7）
Abstract: Nucleic acid detection kit has the characteristics of high sensitivity, specificity and speediness, is widely used in the fields of medical diagnosis, biomedicine and food detection, etc. And it is the technology hotspot of competitive research in various countries, and also the hot field of global concern. Through patent retrieval and analysis for the nucleic acid detection kit，the key indicators of this field are discussed, including the distribution of global / Chinese patent applications, major competing countries, countries of origin and target of patent technology, major applicants, etc. The technology development and innovation trend and the competition situation and development status in this field are disclosed, aiming at inspiring the scientific and technological innovation in China.
Key words: nucleic acid detection ; kit; patent analysis; development trend
引用本文：屈缨虹，罗啸，谢楠，等. 核酸检测试剂盒专利技术发展态势研究[J].化学试剂，2020, 42（7）:749-754.
新型7-甲基-5,6,7,8-四氢-3H-吡啶并[4',3':4,5]噻吩并[2,3-d]嘧啶酮类Schiff碱的合成及抗肿瘤活性研究
李吉莹1，曾慧君2，陈慧琼3，韩潇*1
(1.长江职业学院, 湖北 武汉 430074; 2.武汉食品化妆品检验所, 湖北 武汉 430012;3.武汉爱民制药股份有限公司, 湖北 鄂州 436070)
摘要:以1-甲基-4-哌啶酮为原料，经过Gewald、成环、缩合等反应合成了14个新7-甲基-5,6,7,8-四氢-3H-吡啶并[4',3':4,5]噻吩并[2,3-d]嘧啶酮类Schiff碱，其结构经1HNMR和MS进行确证。初步的生物活性结果表明，目标化合物对荷尔蒙依赖型乳腺癌细胞MCF-7和三阴性乳腺癌细胞MDA-MB-231均有抑制活性，半数抑制浓度(IC50)值均达到微摩尔级，其中部分化合物的抗肿瘤活性甚至强于阳性药物5-氟尿嘧啶(5-FU)和他莫昔芬。尤其是3-(二茂铁亚胺基)-7-甲基-5,6,7,8-四氢-3H-吡啶并[4',3':4,5]噻吩并[2,3-d]嘧啶-4-酮对MCF-7和MDA-MB-231这两种乳腺癌细胞均展现出了最强的抑制活性，其IC50分别为10.5和7.1 mmol/L；此外，目标化合物对正常的MCF-10A细胞没有毒性，而5-氟尿嘧啶和他莫昔芬有毒性。
关键词:Gewald反应；氮杂Wittig 反应；四氢-3H-吡啶并[4',3':4,5]噻吩并[2,3-d]嘧啶酮；Schiff碱；合成；抗肿瘤活性
中图分类号：R914 文献标识码：A 文章编号：0258-3283（2020）
Synthesis and Anti-tumor Activity Evaluation of Novel 7-Methyl-5,6,7,8-tetrahydro-3H-pyrido[4',3':4,5]thieno[2,3-d]pyrimidinone Schiff Bases LI Ji-ying1, ZENG Hui-jun2, CHEN Hui-qiong3, HAN Xiao*1 (1.Changjiang Polytechnic, Wuhan 430074, China; 2.Wuhan Institute for Food and Cosmetic Control, Wuhan 430012, China; 3.Wuhan Aimin Pharmaceutical Limited Company, Ezhou 436070, China), Huaxue Shiji, 2020, 42(7)
Abstract:Fourteen novel7-methyl-5,6,7,8-tetrahydro-3H-pyrido[4',3':4,5]thieno[2,3-d]pyrimidinone Schiff bases were designed and synthesized via Gewald, cyclization, condensation reactions using 1-methyl-4-piperidone as the raw material. The structures of these compounds were confirmed by 1HNMR and MS. The anti-tumor activities were evaluated against hormone-dependent breast cancerMCF-7 and triple-negative breast cancer MDA-MB-231 cell lines in vitro. The preliminary biological results showed that these compounds had inhibitory activities against both MCF-7 and MDA-MB-231 with micromolar value of the half maximal inhibitory concentration (IC50), and some of them exhibited activities better than the positive drugs 5-fluorouracil (5-FU) and tamoxifen. Specifically, 3-(ferrocenyl)-7-methyl-5,6,7,8-tetrahydro-3H-pyrido[4',3':4,5]thieno[2,3-d]pyrimidin-4-one showed the greatest potency against both MCF-7 and MDA-MB-231, and its IC50 was 10.5 and 7.1 mmol/L, respectively. Additionally, all compounds were nontoxic to health MCF-10A cells, while 5-FU and tamoxifen showed essential toxicity.
Key words: Gewald reaction; aza-Wittig reaction;tetrahydro-3H-pyrido[4',3':4,5]thieno[2,3-d] pyrimidin-4-one; Schiff bases; synthesis;anti-tumor activity
引用本文：李吉莹，曾慧君，陈慧琼，等.新型7-甲基-5,6,7,8-四氢-3H-吡啶并[4',3':4,5]噻吩并[2,3-d]嘧啶酮类Schiff碱的合成及抗肿瘤活性研究[J]. 化学试剂，2020，42（7）:755-760.
灭幼脲·阿维菌素超低容量喷雾油剂的制备与活性测试
韦昆1，王晓宇1，刘琴1，李兴忠2，罗会*2
（1. 贵州大学 精细化工研究开发中心，贵州 贵阳 550025；2. 贵州省农业科学院果树科学研究所，贵州 贵阳 550006）
摘要：采用交叉筛选法，从有机溶剂、助剂等方面对配方进行筛选，制备灭幼脲·阿维菌素超低容量喷雾油剂并表征其基本性质，该药剂具有良好的低温稳定性、铺展润湿性，雾滴分散均匀。并通过室内活性试验以及田间生物活性试验，评价了灭幼脲·阿维菌素超低容量喷雾油剂对荔枝蒂蛀虫的防治效果。实验结果表明，灭幼脲·阿维菌素超低容量喷雾油剂对荔枝蒂蛀虫均有良好的防治效果，且优于对照商品药。同时，该油剂是一款适合植保无人机喷施的专用剂型。
关键词：灭幼脲；阿维菌素；超低容量喷雾油剂；植保无人机；荔枝蒂蛀虫；田间药效试验
中图分类号：S436.67 文献标识码：A 文章编号：0258-3283（2020）07--
Preparation and Activity Test of Chlorbenzur on Abamectin ULV Spray Oil Agent WEI Kun1, WANG Xiao-yu1, LIU Qin1, LI Xing-zhong2, LUO Hui*2 (1. Center for R&D of Fine Chemicals, Guizhou University, Guiyang 550025, China; 2.Guizhou Fruit Institute, Guizhou Academy of Agricultural Sciences, Guiyang 550006, China), Huaxue Shiji, 2020, 42(7)
Abstract: The cross screening method was used to screen the formula from the aspects of organic solvents and auxiliaries to prepare chlorbenzur on abamectinultra-low volume(ULV) spray oil agent and testits basic properties. The oil agent possesses excellent cold storage stability, spreading wettability and spray droplets are evenly distributed. Meanwhile, the effects of chlorbenzur on abamectin ULV spray oil agent on conopomorphasinens is bradley were evaluated by laboratory bioactivity tests and field efficacy trials. The results showed that it has good control effect on conopomorphasinens is bradley, indoor activity is 100% and field control rate is 87.5%, and superior to commercial drugs. And the ultra-low capacity spray oil agent developed is a special dosage form suitable for the spraying of unmanned aerial vehicle(UAV) for plant protection.
Key words: chlorbenzuron; abamectin; ltra-low capacity spray oil agent; plant protection uav; conopomorphasinensis bradley; field efficacy trials
引用本文：韦昆，王晓宇，刘琴，等. 灭幼脲•阿维菌素超低容量喷雾油剂的制备与活性测试[J].化学试剂，2020，42（7）：761-766.
生物膜电极的制备及其在抗菌药物有效性检测中的应用
马烨，何迪，陈立志，王晶晶，王超，刘畅*
（锦州医科大学 药学院，辽宁 锦州 121000）
摘要：首先采用电聚合法制备了聚中性红修饰玻碳电极（PNR/GCE），在此基础上，以壳聚糖（CS）为成膜材料，石墨烯（GR）为导电纳米材料，通过掺杂方式将模型微生物E. coli固定于PNR/GCE上，制备生物膜电极GR/CS/E. coli/PNR/GCE。采用正交实验和方差分析考察GR浓度、CS浓度和E. coli浓度3个因素对GR/CS/E. coli/PNR/GCE性能的影响。继而借助中性红可作为电子媒介体的特性，通过考察E. coli活性与抗菌药物浓度的关系构建一种新型体外药效检测方法，用以快速检测抗菌药物有效性。GR终浓度0.50 mg/mL，CS终浓度0.75%（w/v%），E. coli终浓度0.50 g/mL为电极制备的最佳条件。将最优条件下制备的GR/CS/E. coli/PNR/GCE应用于庆大霉素、左氧氟沙星、头孢曲松钠、哌拉西林钠及万古霉素5种抗菌药物的有效性测定，其中前4种抗菌药物对E. coli的10%抑菌浓度（IC10）分别为15.81、19.62、65.74、62.47 mg/L，而针对革兰氏阳性菌的万古霉素对E. coli基本无抑制作用。上述所得结果与经典的纸片扩散法所得结果具有良好的相关性。
关键词：聚中性红；修饰电极；微生物固定化；生物膜电极；抗菌药物有效性检测
中图分类号： O657.1文献标识码：A 文章编号：0258-3283（2020）--
Preparation of Biofilm Electrode and Application in the Detection of Antimicrobial Efficacy MA Ye, HE Di, CHEN Li-zhi, WANG Jing-jing, WANG Chao, LIU Chang*(College of Pharmacy, Jinzhou Medical University, Jinzhou 121000, China), Huaxue Shiji, 2020, 42( ), ～
Abstract: Firstly, poly neutral red modified glassy carbon electrode (PNR/GCE) was prepared by electropolymerization. On this basis, chitosan (CS) as a film-forming material and grapheme (GR) as a conductive nanomaterial, biofilm electrode GR/CS/E. coli/PNR/GCE was prepared by immobilization of model microorganism E. coli to PNR/GCE by doping method. Orthogonal design and analysis of variance were used to investigate the influence of three factors, such as GR concentration, CS concentration and E. coli concentration, on the GR/CS/E. coli/PNR/GCE performance. Then a new method for rapid detection of antimicrobial efficacy in vitro was constructed where NR as an electron mediator was employed in investigating the relationship between the activity of E. coli and the concentration of antimicrobials. The optimum conditions for electrode preparation were as follows: the final concentrations of GR, CS and E. coli were 0.5 mg/mL, 0.75% (w/v%), 0.50 g/mL, respectively. The prepared GR/CS/E. coli/PNR/GCE under the optimal conditions was applied to detect the efficacies of gentamycin, levofloxacin, ceftriaxone sodium, piperacillin sodium and vancomycin, which antimicrobial agents mentioned above, such as gentamycin, levofloxacin, ceftriaxone sodium and piperacillin sodium, showed 10% inhibition on E. coli with the inhibiting concentration (IC) of 15.81, 19.62, 65.74, 62.47 mg/L, respectively. In contrast, vancomycin, as an antibiotic against gram-positive bacteria, had little inhibitory effect on E. coli cells. The results obtained above were in good correlation with the results obtained by classical disk diffusion method.
Key words: poly neutral red; modified electrode; immobilization of microorganisms; biofilm electrode; antimicrobial efficacy detection
引用本文：马烨, 何迪, 陈立, 等. 生物膜电极的制备及其在抗菌药物有效性检测中的应用[J]. 化学试剂, 2020, 42(7): 767-772.
聚乙烯亚胺改性氧化石墨对水中铜离子的吸附性能研究
闫慧君*，牟子剑，王爽，张宏坤，张小善，姜艳丽
(哈尔滨学院 食品工程学院，黑龙江 哈尔滨 150086)
摘要：通过将聚乙烯亚胺(PEI)嫁接到氧化石墨(GO)表面，制备出聚乙烯亚胺改性氧化石墨(PEI-GO)复合物。通过FT-IR、TEM、XPS、TGA和拉曼光谱等对其进行表征，结果表明PEI成功嫁接到GO表面上，同时研究了PEI-GO对水中Cu(II)的吸脱附性能。PEI-GO对Cu(II)的吸附动力学可以用准二级动力学方程描述，吸附等温线可用Langmuir方程模拟，吸附过程呈现单层吸附现象，PEI-GO在pH5、5mg/L的Cu(II)溶液中最大吸附容量可达205 mg/g。经过5次循环再生实验发现去除率仍保持58.3%，结果表明PEI-GO对水中Cu(II)去除效果明显，是一种优异的吸附剂。
关键字：聚乙烯亚胺；改性；氧化石墨；Cu(II)；吸附性能
中图分类号：O611.64 文献标识码：A 文章编号：0258-3283(2020)
Adsorption Property of Polyethyleneimine Modified Graphite Oxide for Cu(II) YAN Hui-jun*, MOU Zi-jian, WANG Shuang, ZHANG Hong-kun, ZHANG Xiao-shan, JIANG Yan-li (College of Food Engineering, Harbin University, Harbin 150086, China), HuaxueShiji, 2020, 42(7)
Abstract: Polyethyleneimine (PEI) was grafted onto the surface of graphite oxide (GO) by oxidizing graphite, and polyethyleneimine modified graphite oxide (PEI-GO) composite was prepared. The structure and surface properties of the composites were characterized by FT-IR, TEM, XPS, TGA and Raman. PEI was successfully grafted on the surface of GO. Meanwhile, its adsorption and desorption capability for Cu(II) was investigated. Its adsorption process complies with the Langmuir isothermal adsorption model and pseudo-second-order kinetic model. It also presents monolayer adsorption. The maximum adsorption capability of Cu(II) is 205 mg/g in 5 mg/L Cu(II) solution at pH 5. After four consecutive adsorption/desorption cycles, the removal rate still remains 58.3%. Results show PEI-GO is a good adsorbent for Cu(II) with promising potential applications for the removal of Cu(II) ions from aqueous solution.
Key words: polyethyleneimine; modified; graphite oxide; Cu (II); adsorption capability
引用本文：闫慧君，牟子剑，王爽，等.聚乙烯亚胺改性氧化石墨对水中铜离子的吸附性能研究[J].化学试剂，2020，42（7）：773-779.
玉米芯活性炭吸附重金属离子的研究
糜志远，肖瑞，张佳*，杨慧杰，张紫薇，邵君前，陈子良，郑婉榕，余庆节
（湖北工业大学 生物工程与食品学院，湖北 武汉 430064）
摘要：以玉米芯为实验原材料，制得活性炭，探究活性炭在不同的重金属浓度、pH以及不同的吸附时间下对重金属的吸附效果，并利用正交试验探究活性炭的最佳吸附条件。结果显示：重金属Pb的最佳吸附浓度为5 μg/mL，最佳吸附时间为5 h，最佳溶液pH 5；重金属Hg的最佳吸附浓度为30 μg/mL，最佳吸附时间为5 h，最佳溶液pH 1；重金属Cd的最佳吸附浓度为5 μg/mL，最佳吸附时间为5 h，最佳溶液pH 5。本工艺方法操作简单快捷、原料来源广泛、制作成本低，且制备的活性炭对Pb、Hg、Cd等重金属离子具有良好的吸附能力，以便于广泛运用。
关键词：活性炭；浓度；时间；pH；Pb；Hg；Cd
中图分类号：TQ424.1 文献标识码：A 文章编号：0258-3283（2020）
Adsorption of Heavy Metal Ions by Corn Cob Activated Carbon MI Zhi-yuan, XIAO Rui, ZHANG Jia*, YANG Hui-jie, ZHANG Zi-wei, SHAO Jun-qian, CHEN Zi-liang, ZHENG Wan-rong, YU Qing-jie (School of Bioengineering and Food, Hubei University of Technology, Wuhan 430064, China), Huaxue Shiji, 2020, 42(7)
Abstract: Activated carbon was prepared with corn cob as the raw material, to explore the adsorption effect of activated carbon on heavy metals at different concentrations, pH and different adsorption time, and to explore the optimal adsorption conditions of activated carbon by orthogonal experiment. The best adsorption concentration of Pb was 5μg/mL, the best adsorption time was 5h, and the best solution pH was 5. The optimal adsorption concentration of heavy metal Hg was 30μg/mL, the optimal adsorption time was 5h, and the optimal solution pH was 1. The optimal adsorption concentration of heavy metal Cd was 5μg/mL, the optimal adsorption time was 5h, and the optimal solution pH was 5. The process is simple and rapid, the source of raw materials is wide, the production cost is low, and the prepared activated carbon has good adsorption capacity for heavy metal ions such as lead, mercury and cadmium, so as to be widely used.
Key words: activated carbon；concentration；time；pH；Pb；Hg；Cd
引用本文：糜志远，肖瑞，张佳, 等. 玉米芯活性炭吸附重金属离子的研究[J]. 化学试剂, 2020, 42(7):780-785.
水热法制备荧光二硫化钼量子点在三价铁离子检测中的应用
王琦1，许静静1，张秀莉2，李菁菁*1,2，徐凯*1,2
(1. 徐州医科大学 医学影像学院，江苏 徐州 221004；2.徐州医科大学附属医院 影像科，江苏 徐州2 21002）
摘要：采用谷胱甘肽作为硫源，钼酸钠作为钼源，利用反应釜高温水热法制备二硫化钼量子点（MoS2QDs），显微镜（AFM、TEM）、荧光光谱及紫外光谱显示其为单层结构，粒径约为5.26 nm，可发出深蓝荧光，最大激发、发射波长分别位于310、410 nm处，此MoS2QDs制备方法简单，所合成MoS2QDs具有优异的荧光性质。Fe3+对MoS2QDs具有明显的荧光淬灭作用，当Fe3+的浓度范围为1～500 nmol/L时，Fe3+浓度与MoS2QDs荧光强度之间线性相关性较好（线性方程为：y = 1.2775+0.0028 x, R2= 0.9948），检测限约为3.4 nmol/L。以此作为理论基础，构建了一种新的Fe3+检测方法，该检测方法简单、迅速，不产生环境有害物质，可用于自然水系中Fe3+的检测，为环境检测提供新的技术支持。
关键词：二硫化钼量子点；荧光；三价铁离子检测；谷胱甘肽；水热法
中图分类号：X832 文献标识码：A 文章编号：0258-3283（2020）
Hydrothermal Fabrication of Fluorescent MoS2 Quantum Dots and Application in the Detection of Fe3+
WANG Qi1, XU Jing-jing1, ZHANG Xiu-li2, LI Jing-jing *1, 2 ,XU Kai *1, 2(1. School of Medical Imaging, Xuzhou Medical University, Xuzhou 221004, China; 2.Department of Radiology, Affiliated Hospital of Xuzhou Medical University, Xuzhou 221002, China), Huaxue Shiji, 2020, 42(7)
Abstract: A facile hydrothermal approach was developed for the preparation of molybdenum disulfide quantum dot (MoS2 QDs) with glutathione as the sulfur source and sodium molybdate as the molybdenum source. AFM, TEM, fluorescence spectrum and UV showed that MoS2 QDs was a monolayer structure with a particle size of about 5.26 nm, which could emit dark blue fluorescence, and the maximum excitation and emission wavelength were located at 310 nm and 410 nm respectively .This is a simple method for the preparation of MoS2 QDs andthe synthesized MoS2 QDs had excellent fluorescence properties. Fe3+ ions displayed obvious fluorescence quenching ability on the fluorescence of MoS2 QDs and the quenching content was linearly related to Fe3+concentrations (1 ~ 500 nmol/L). The linear regression equation was y= 1.2775+0.0028 x, the correlation coefficient R2=0.9948, and the detection limit was 3.41 nmol/L. Based on the fluorescence quenching of MoS2 QDs by Fe3+ ions, a new method for Fe3+ions detection was constructed and implemented. The fabricated method was harmless, simple and quick, which can be used for the detection of Fe3+ in the real environment water, providing a new technical support for environment analysis.
Key words: molybdenum disulfide quantum dot; fluorescence; ferric ion detection; glutathione; hydrothermal method
引用本文：王琦，许静静，张秀莉，等. 水热法制备荧光二硫化钼量子点在三价铁离子检测中的应用[J].化学试剂，2020, 42（7）:786-790.
聚苯胺衍生的多孔碳纳米管对罗丹明B的吸附性能研究
赵德1，陈国举1，李亦婧2，卢晓锋2，牛盼红*2,3，郭勇*2
（1. 金川集团股份有限公司 镍钴资源综合利用国家重点实验室，甘肃 金昌 737100；2. 中国科学院兰州化学物理研究所 西北植物资源化学重点实验室 甘肃省天然药物重点实验室，甘肃 兰州 730000；3. 中国科学院大学，北京 100049）
摘要：以聚苯胺为碳源，通过高温热解和KOH化学活化法制备了多孔聚苯胺碳纳米管（PPN），将其用于吸附罗丹明B（RhB）。PPN具有大的比表面积（2055.30 m2/g）和孔体积（1.32 cm³/g），对RhB的吸附容量高达433.30mg/g。将Langmuir和Freundlich等温吸附模型用于研究PPN吸附RhB过程。实验结果表明，吸附模型更符合Langmuir等温吸附模型，属于均相表面的单分子层可逆吸附。准一级动力学、二级动力学和内颗粒扩散模型研究吸附动力学过程，PPN对RhB的吸附符合准二级动力学模型。PPN用于RhB吸附，在30次循环使用后，仍然表现出优异的回收率（86.9%），表明PPN是一种高效并且可以循环使用的吸附材料，具有用于废水中移除RhB的潜力。
关键词：多孔碳纳米管；罗丹明B；固相萃取；聚苯胺；循环利用；吸附剂
中图分类号：X751 文献标识码：A 文章编号：0258-3283（2020）--
Investigation on the Adsorption of Rhodamine B by Polyaniline Derived Porouscarbon Nanotubes ZHAO De1, CHEN Guo-jv1, LI Yi-jing2, LU Xiao-feng2, NIU Pan-hong*2,3, GUO Yong*2 (1. State Key Laboratory of Nickel and Cobalt Resources Comprehensive Utilization, Jinchuan Group Co., Ltd., Jinchang 737100, China; 2. Key Laboratory of Chemistry of Northwestern Plant Resource and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Gansu 730000, China; 3. University of Chinese Academy of Sciences, Beijing 100049, China), Huaxue Shiji, 2020, 42(7), ～
Abstract: Using polyaniline as carbon source, porous polyaniline nanotube (PPN) was prepared via high-temperature pyrolysis and further KOH chemical activation method, which was employed in the adsorption of Rhodamine B (RhB). PPN adsorbent exhibited a large specific surface area (2055.30 m2/g) and pore volume (1.32 cm/g), and its adsorption capacity for RhB was as high as 433.30 mg/g. Langmuir and Freundlich isothermal adsorption models were used to investigate the adsorption behavior of RhB by PPN. The results were more consistent with the Langmuir isotherm adsorption model, which was ascribed as reversible adsorption of monolayer on homogeneous surface. Three kinetics models including pseudo-first-model, pseudo-second-model and internal particle diffusion model were employed to investigate the adsorption process of RhB. The adsorption behavior of RhB by PPN was in accordance with the pseudo-second-model. After 30 cycles of use, PPN still showed a good extraction recovery (86.9%), indicating that PPN was an efficient and recyclable adsorbent with the expectable potential to remove RhB from wastewater.
Key words: porous carbon nanotube; rhodamine B; solid phase extraction; polyaniline; regeneration; adsorbent
引用本文：赵德,, 陈国举,, 李亦婧, 等. 聚苯胺衍生的多孔碳纳米管对罗丹明B的吸附性能研究[J]. 化学试剂,2020, 42(7): 791-796.
重金属污染物诱发胃癌作用的研究进展
任婷，赵丽娇*，钟儒刚
（北京工业大学 生命科学与生物工程学院 环境与病毒肿瘤学北京市重点实验室, 北京 100124）
摘要：癌症是严重威胁人类生活和健康的重大疾病。由于胃部解剖学位置特点及其具有的与其他器官完全不同的酸性环境，重金属污染物在诱导胃癌发生中的作用必须得到重视。大量流行病学研究显示，土壤、灌溉水、饮用水和食品中重金属含量与胃癌发病率之间存在正相关性。重金属元素通过破坏胃粘膜屏蔽、导致胃上皮及内皮组织产生过度氧化应激反应、干扰细胞信号通道和基因表达、与生物大分子相结合导致蛋白质和DNA分子的损伤、破坏DNA损伤的修复作用、以及影响基因的表观遗传学作用等机理使细胞发生恶性转化。机理分析发现，重金属可以和幽门螺旋杆菌协同作用，提高胃癌的发病率。因此，冶金、矿业、材料、化工和食品等产业，农田土壤和水质修复工作等在涉及重金属污染物的问题时应该有更严格和全面的措施。
关键词：重金属；胃癌；致癌机理；协同作用；癌症防治
中图分类号：X503 文献标识码： A 文章编号：0258-3283（2020）
Progress in the Effects of Heavy Metal Pollutants on Gastric Cancer REN Ting, ZHAO Li-jiao*, ZHONG Ru-gang(Beijing Key Laboratory of Environmental & Viral Oncology, College of Life Science and Bioengineering, Beijing University of Technology, Beijing 100124, China ), Huaxue Shiji, 2020,42(7)
Abstract：Cancer is a kind of serious diseases threatening human life and health. Due to the anatomic location of stomach and its acid environment which is completely different from other organs, the role of heavy metal pollutants in the induction of gastric cancer must be taken seriously. A large number of epidemiological studies have shown that there is a positive correlation between heavy metal content in soil, irrigation water, drinking water and/or food with the incidence rate of gastric cancer. Heavy metals cause malignant transformation of cells by destroying the barrier of gastric mucosa, causing excessive oxidative stress reaction in gastric epithelium and endothelium, interfering with cell signal channels and gene expression, combining with biological macromolecules, leading to damage of protein and DNA molecules, damaging the repair effect of DNA damage, and affecting the epigenetic effect of genes. The heavy metals can synergy with Helicobacter pylori and increase the incidence rate of gastric cancer. Therefore, in metallurgy, mining, materials, chemical industry, food and other industries, farmland soil and water quality remediation work should have more strict and comprehensive measures when it comes to heavy metal pollutants.
Key words：heavy metals; gastric cancer; carcinogenic mechanism; synergism; cancer prevention
引用本文：任婷，赵丽娇，钟儒刚. 重金属污染物诱发胃癌作用的研究进展[J].化学试剂，2020，42（7）：797-802.
基于叶酸-壳聚糖偶联物及其衍生物在载药体系的应用研究进展
陆钊*1a，张怡之1a，胡志刚2，张俊伟3，丁馨怡1a，刘茂顺1b，刘佳豪1b
1. 吉林医药学院 a. 药学院，b. 检验学院，吉林 吉林 132000；2. 吉林石化分公司电石厂，吉林 吉林 132000；3. 延边大学 药学院，吉林 延边 133000）
摘要：叶酸具有受体靶向性、无免疫原性和便于修饰等优异性能，壳聚糖及其衍生物具有良好的生物相容性、粘附性、生物可降解性等优异性能，叶酸-壳聚糖及其衍生物的偶联物兼备二者的优点，在生物医学领域具有广阔的应用前景。综述了国内外学者近几年关于叶酸-壳聚糖偶联物在载药体系方面的研究进展，最后结合叶酸-壳聚糖偶联物在制备方法、体内释放、未来研究方向等方面进行了总结和展望。
关键词：叶酸；壳聚糖；药物载体；脂质体；聚乳酸-羟基乙酸共聚物；石墨烯；碳纳米管
中图分类号：R94 文献标识码：A 稿件编号：0258-3283（2020）--
Progress on Application of Folate-Chitosan Conjugates and Derivatives in Drug-Loaded Systems LU Zhao*1a, ZHANG Yi-zhi1a, HU Zhi-gang2, ZHANG Jun-wei3, DING Xin-yi1a, LIU Mao-shun1b, Jia-hao1b (1a. School of Pharmacy, 1b. School of Inspection, Jilin Medical University, Jilin 132000, China; 2. Carbide Plant of Jilin Petrochemical Company, Jilin 132000, China; 3. School of Pharmacy, Yanbian University, YanBian 133000, China ), Huaxue Shiji, 42( ), ～
Abstract:Folic acid has excellent properties such as receptor targeting, non-immunogenicity, and easy modification. Chitosan and its derivatives also have good properties such as biocompatibility, adhesion, and biodegradability. The folic acid-chitosan and its derivatives has the advantages of chitosan and folic acid, and has broad application prospects in the field of biomedicine. Therefore, this article reviews the research progress of folic acid-chitosan conjugates in drug loading systems in recent years and summarized and prospected in terms of preparation methods, in vivo release, and future research directions.
Key words：folic acid；chitosan；drug carrier；liposomes; PLGA; grapheme; carbon nanotubes
引用本文：陆钊,, 张怡之,, 胡志刚, 等. 基于叶酸-壳聚糖偶联物及其衍生物在载药体系的应用研究进展[J]. 化学试剂, 2020, 42(7): 803-812.
UPLC-PDA法测定不同茎色黄芪中花青素的含量及变化
贺润丽，韩毅丽*，王亚丽，张慧玲，梁颖
（山西中医药大学 中药与食品工程学院，山西 晋中 030619）
摘要：采用UPLC-PDA法测定不同茎色黄芪中矢车菊素、飞燕草素的含量，比较不同采收期、放置期黄芪药材中矢车菊素、飞燕草素含量的变化。采用Waters AcQuity UPLC®BEH-C18（100 mm × 2.1 mm，1.7μm）色谱柱，流动相为乙腈-0.1%甲酸水溶液，梯度洗脱，流速0.3 mL/min，柱温30 ℃，检测波长530 nm。矢车菊素、飞燕草素线性范围分别为3.58～28.64 µg/mL（r =0.9998）、2.17～17.36 µg/mL（r =0.9997），平均回收率( n = 6)分别为98.57% ( RSD = 2.6% )和99.53% ( RSD = 0.65%)。不同采收期紫茎黄芪中矢车菊素和飞燕草素含量差异较大，但六月下旬后矢车菊素和飞燕草素的总含量基本稳定，药材放置4个月后飞燕草素和矢车菊素含量下降率分别为26.77%和21.36%。绿茎黄芪中未检测到矢车菊素和飞燕草素。该方法简便快捷，适用于黄芪中花青素的含量测定研究，为黄芪花青素合成相关基因分析及黄芪药材栽培技术的改进提供了依据。
关键词：UPLC-PDA；黄芪；花青素；矢车菊素；飞燕草素；采收期；放置期；含量变化
中图分类号： 文献标识码：A 文章编号：0258-3283（2020）
Determination of Anthocyanins Content in Different Colored Stems Astragalus by UPLC-PDA HE Run-li, HAN Yi-li*, WANG Ya-li, ZHANG Hui-ling, LIANG Ying( School of Traditional Chinese Medicine and Food Engineering, Shanxi University of Traditional Chinese Medicine, Jinzhong 030619, China), Huaxue Shiji, 2020, 42(7)
Abstract: To establish an UPLC-PDA method for the determination of cyanidin and delphinidin in Astragalus of different colored stems from different gathering and storage periods. Waters AcQuity UPLC®BEH－C18（100 mm × 2.1 mm，1.7μm) was adoped with a mobile phase of acetonitrile－0.1% formic acid water, the separation was carried out with a gradient program at a flow rate of 0.3 mL·min-1,column temperature was 35 ℃ and detection wavelength was 260 nm. cyanidin and delphinidin showed good linearity in the ranges of 3.58 ～ 28.64 µg/mL（r =0.9998）and 2.17～17.36 µg/mL（r =0.9997） with average recoveries of 98. 57% ( RSD = 2.6% ) and 99. 53% ( RSD = 0.65% ) , respectively． The contents of cyanidin and delphinidin in Astragalus of purple stems from different gathering periodst marked difference, but in late June, the total contents of cyanidin and delphinidin were stable, four months after harvesting, the decrease rate of the content of delphinidin and cyanidin were 26.77% and 21.36%, respectively. Cyanidin and delphinidin were not detected in Astragalus of green stems. The method is simple, rapid for determination the contents of anthocyanins in Astragalus，and can be used for analyzing the synthetic genes of anthocyanins and cultivation techniques of Astragalus better habitat and gathering periods of Astragali Radix．
Key words: UPLC-PDA; Astragali Radix; Anthocyanins; cyanidin; delphinidin; gathering periods; storage periods; changes of contents
引用本文：贺润丽, 韩毅丽, 王亚丽, 等. UPLC-PDA法测定不同茎色黄芪中花青素的含量及变化[J]. 化学试剂, 2020, 42(7):813-817.
选择性薄膜电导率法测定水中总有机碳的方法学研究
周小新，孟元华，周虹，刘文卫*
（无锡市疾病预防控制中心，江苏 无锡 214023）
摘要：建立饮用水中总有机碳的选择型薄膜电导率检测法。水样中有机物被氧化生成的CO2，从样品水一侧穿过对CO2有选择性的渗透膜，进入到仅含去离子水的另一侧。电离反应生成碳酸氢根离子与氢离子，使水的电导率升高，根据此时的电导率升高变化来表征CO2的浓度。结果 总有机碳在0.20 ～10.0 mg/L线性范围内回归方程为y=0.963x+0.0460，线性相关系数R﹥0.999，方法检出限为0.20 mg/L，其中纯水的加标回收率为90.0%～110%，相对标准偏差（RSD）为0.83%～2.50%；末梢水的加标回收率为99.8%～108%，相对标准偏差为0.23%～0.87%；水源水的加标回收率为91.5%～107%，相对标准偏差为0.15%～0.88%。方法灵敏度高、准确度好、检出限低、而且稳定好，适合生活饮用水及其水源水、涉水产品浸泡水中总有机碳的测定，并在多领域进行了推广应用，有望成为行业标准。
关键词：水；总有机碳；选择性薄膜电导率检测法；测定；方法学
中图分类号：O652.1 文献标识码：A 文章编号：0258-3283（2020）--
Methodology for Determination of Total Organic Carbon in Water by Membrane Conductivity Detection ZHOU Xiao-xin, MENG Yuan-hua, ZHOU Hong, LIU Wen-wei*(Wuxi Center of Disease Control and Prevention, Wuxi 214023, China), Huaxue Shiji, 42(7), ～
Abstract: Establish a membrane conductivity detection method of TOC in drinking water. The CO2 formed by the oxidation of organic matter in the water sample passes through the permeable membrane selective to CO2 from the water side of the sample to the other side containing only deionized water. The ionization reaction generates hydrogen carbonate ions and hydrogen ions to increase the conductivity of the water, and characterizes the concentration of CO2 according to the change in conductivity at this time. The total organic carbon in the linear range of 0.20～10.0mg/L has a regression equation of y=0.963x+0.0460, the linear correlation coefficient R>0.999, the lowest detection mass concentration of the method was 0.20 mg/L, and the spiked recovery rate of pure water was 90.0%～110%, relative standard deviation (RSD) was 0.83%～2.50%，spiked recovery of peripheral water was 99.8%～108%, relative standard deviation (RSD) was 0.23%～0.87%. The standard recovery was 91.5% ～ 107%, and the relative standard deviation (RSD) was 0.15% ～ 0.88%. The method has high sensitivity, good accuracy, low detection limit and good stability. It is suitable for the determination of total organic carbon in drinking water and water source and wading products. It has been promoted and applied in many fields and is expected to become an industry standard.
Key words: water；total organic carbon；membrane conductivity detection；determination；methodology
引用本文：周小新, 孟元华, 周虹, 等. 选择性薄膜电导率法测定水中总有机碳的方法学研究[J]. 化学试剂, 2020, 42(7): 818-821.
旋光法快速测定D-阿洛酮糖的实验研究
邢敏钰1，冉淦桥1，殷红1，韩姗姗2，张红艳2，张强*1
（1. 陕西省生物农业研究所，陕西 西安 710034；2. 陕西省酶工程技术研究中心，陕西 西安 710600）
摘要：采用旋光法建立D-阿洛酮糖的快速检测方法，并对方法进行验证。确定旋光法快速定量检测D-阿洛酮糖的条件，并对方法的线性范围、准确度、精密度以及重复性进行验证。尽管D-阿洛酮糖的旋光度受温度影响，在10 ~ 40 ℃范围内，随温度升高而升高。但是在同一温度条件下，0.01 ～ 0.3 g/mL浓度范围内，D-阿洛酮糖浓度与旋光值具有良好的线性关系（线性回归方程为y=3.77384x+0.01935，相关系数（R2）为0.99972）。随机测定3个不同浓度D-阿洛酮糖溶液的旋光值，通过回归曲线计算得到理论浓度，将理论浓度与实际浓度进行单因素方差分析，不存在显著性差异（p>0.05），说明方法具有较好的准确度。计算平行样品的相对标准偏差（RSD），发现精密度实验和重复性试验的RSD值均小于5%。因此，方法具有较好的精密度和重复性。方法在0.01 ～ 0.3 g/mL浓度范围内线性良好，且具有较好的准确度、精密度和重复性，能够作为一种快速、简便、准确的定量检测D-阿洛酮糖方法。
关键词：旋光法；D-阿洛酮糖；定量检测；准确度；精密度；重复性
中图分类号：TS247 文献标识码：A 文章编号：0258-3283（2020）--
Rapid Determination of D-psicose by Polarimetry XING Min-yu1, RAN Gan-qiao1, YIN Hong1, HAN Shan-shan2, ZHANG Hong-yan2, ZHANG Qiang*1 (1.Bio-Agriculture Institute of Shaanxi, Xi’an 710034, China; 2.Enzyme Engineering Research Center of Shaanxi Province, Xi’an 710600, China), Huaxue Shiji, 2020, 42(7), ～
Abstract: A rapid detection method was established for D-psicose by polarimetry, and the method was verified. The experimental conditions were optimized for verifying the linear range, accuracy, precision and repeatability of the method. The results showed that the optical rotation of D-psicose was affected by temperature. In the range of the temperature (10 ~ 40 ℃), the optical rotation of D-psicose increased with the increasing of the temperature. However, at the same temperature conditions, there was a good linear relationship in the range of 0.01 ~ 0.3 g/ml between the concentration of D-psicose and the optical rotation (the regression equation: y=3.77384x+0.01935, R2= 0.99972). The optical rotation values of D-psicose solutions with three concentration gradients were randomly measured, and the theoretical concentrations of D-psicose solutions were calculated by the regression equation. One-way analysis of variance results (p>0.05) showed that there was no significant difference between the theoretical concentration and the actual concentration, indicating that the method has a good accuracy. The precision and repeatability of this method were evaluated and it turned out that the relative standard deviation (RSD) was less than 5%. Therefore, this method has better precision and repeatability. The linearity of the method was well in the concentration range of 0.01 ~ 0.3 g/mL and has good accuracy, precision and repeatability. It is a rapid, simple and accurate method for the quantitative determination of D-psicose.
Key words：polarimetry; D-psicose; quantitative detection; accuracy; precision; repeatability
引用本文：邢敏钰, 冉淦桥, 殷红, 等. 旋光法快速测定D-阿洛酮糖的实验研究[J]. 化学试剂, 2020, 42(7) :822-827.
电位滴定法测定原油酸值的不确定度评定
王家兴*，张雁玲
(中国石化大连石油化工研究院，辽宁 大连 116045)
摘要：利用电位滴定法对原油中的酸值进行测定，对酸值试验结果进行了不确定度评定，建立酸值不确定度评定的计算模型，分析和计算了试验过程中影响酸值测量结果的不确定度分量，进而给出原油酸值的不确定度，原油酸值的测定结果为0.63 mg/g ，其扩展不确定度为0.01 mg/g（置信因子k=2），原油酸值重复性试验是影响该方法不确定度的主要因素，重视原油试样及氢氧化钾异丙醇的滴定过程对不确定度产生的影响，原油酸值测定中，应重点从这2个方面加以改进，提高酸值测量结果的准确性。
关键词：原油；酸值；电位滴定法；不确定度；评定
中图分类号：TB99 文献标识码：A 文章编号：0258-3283（2020）
Evaluate the Uncertainty of the Acid Number of Crude oil by the Potentiometric Titration Test Method WANG Jia-xing, ZHANG Yan-ling(Dalian Research Institute of Petroleum and Petrochemical of Sinopec, Dalian 116045, China), Huaxue Shiji, 2020, 42(7)
Abstract：The acid number of crude oil is determined by potentiometric titration method. The uncertainty of the acid number are evaluated. The calculation model of the acid number uncertainty is established. The uncertainty components affecting the acid number measurement results during the test are analyzed and calculated. The uncertainty of the acid number of crude oil is further given. The determination result of the acid number of crude oil is 0.63 mg/g, and its expanded uncertainty is 0.01 mg/g (confidence factor k=2). The repeatability test of crude oil acid number is the main factor affecting the uncertainty of the method. Attention should be paid to the influence of the titration process of crude oil sample and potassium hydroxide isopropyl alcohol on the uncertainty. In the determination of crude oil acid number, improvement should be focused on these two aspects to improve the accuracy of the acid number measurement results.
Key words：crude oil; acid number; potentiometric titration; uncertainty; evaluate
引用本文：王家兴，张雁玲. 电位滴定法测定原油酸值的不确定度评定[J].化学试剂，2020，42（7）：828-831.
考马斯亮蓝R250共振光散射光谱法测定壳聚糖含量
许钟元a,d，袁莉b,d，李银华c,d，王振b,d，余梦婷b,d，马卫兴*b,d，陈丽a,e
(江苏海洋大学 a.海洋生命与水产学院，b.药学院，c.化学工程学院，d.江苏省海洋药物筛选重点实验室，e.江苏省海洋资源开发研究院，江苏 连云港 222005)
摘要：壳聚糖为碱性高分子多糖，可广泛应用于各个领域，因此壳聚糖的含量测定至关重要。研究表明，壳聚糖在pH 2.40的Clark-Lubs缓冲溶液中形成质子化的壳聚糖阳离子，再与阴离子染料考马斯亮蓝R250形成离子缔合物，使体系的共振光散射强度显著增强。在325 nm处共振光强度增强值△I与壳聚糖浓度在0.10～0.80 mg/L内呈线性关系，检出限（3S/K）为0.012 mg/L。方法用于壳聚糖胶囊的分析，测定值与变色酸2B褪色分光光度法结果一致。
关键词：壳聚糖；考马斯亮蓝R250；共振光散射（RLS）；离子缔合反应；含量测定
中图分类号：O-31 文献识别码：A文章编号：0258-3283（2020）--
Determination of Chitosan Content by Coomassie Brilliant Blue R250 Resonance Light Scattering Spectroscopy XU Zhong-yuana,d, YUAN Lib,d, LI Yin-huac,d, WANG Zhenb,d, YU Meng-tingb,d, MA Wei-xing*b,d, CHEN Lia,e(a. School of Marine Life and Fisheries, b. School of Pharmacey, c. School of Chemical Engineering Marine Life and Fisheries, d. Jiangsu Key Laboratory of Marine Pharmaceutical School Screening, e. Jiangsu Academy of Marine Resources Development, Jiangsu Ocean University, Lianyungang 222005, China), Huaxue Shiji, 2020, 42(7), ～
Abstract：Chitosan is a basic polymer polysaccharide, which can be widely used in various fields, so the determination of chitosan content is very important. This work shows that chitosan forms protonated chitosan cations in Clark-Lubs buffer solution at pH 2.40, which bonded with coomassie brilliant blue R250(anionic dye) could significantly enhance the intensity of resonance light. The resonance light intensity enhancement value △ I at 325 nm has a linear relationship with the concentration of chitosan within 0.10 ~ 0.80 mg/L, and the detection limit (3s / k)was 0.012 mg/L. The method was used for the analysis of chitosan capsules, and the measured values were consistent with the results of discoloring spectrophotometry of chromotrope 2B.
Key words: chitosan; coomassie brilliant blue R250；resonance light scattering；ion association reaction；content determination
引用本文：许钟元, 袁莉, 李银华, 等. 考马斯亮蓝R250共振光散射光谱法测定壳聚糖含量[J]. 化学试剂，2020, 42(7): 832-835.
丹酚酸A与人血清白蛋白的相互作用研究
朱西挺*，熊晨，周杨，龚忆霖，杨佳浩
（南通大学 化学化工学院，江苏 南通 226019）
摘要：研究药物和血浆中载体蛋白的相互作用对阐明药物在体内的转运、分布、代谢和药效等具有重要的意义。采用荧光光谱和紫外-可见吸收光谱法研究了不同温度下丹酚酸A（Sal A）与人血清白蛋白（HSA）的相互作用机理。研究结果表明，Sal A对HSA的内源荧光有明显的猝灭作用，猝灭过程为静态猝灭，并测定和计算得到不同温度下Sal A与HSA反应的结合常数、结合位点数。分析两者结合过程的热力学数据，表明Sal A和HSA的结合是一种自发的放热过程，且推测出Sal A与HSA之间的作用力为氢键和范德华力。
关键词：丹酚酸A；人血清白蛋白；紫外吸收光谱；荧光光谱
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283（2020）07--
Interaction of Salvianolic Acid A with Human Serum Albumin ZHU Xi-ting, XIONG Chen, ZHOU Yang, GONG Yi-lin, YANG Jia-hao (School of Chemistry and Chemical Engineering, Nantong University, Nantong 226019, China), Huaxue Shiji, 2020, 42(7), ～
Abstract：The interactions between drugs and carrier proteins in blood are important for elucidating the transport, distribution, metabolism and efficacy of drugs in vivo. In this work, fluorescence spectroscopy and UV-Vis absorption spectrometry assays were used to investigate the interaction mechanism of salvianolic acid A (Sal A) and human serum albumin (HSA) at different temperatures. Fluorescence spectroscopy results showed that Sal A may lead to fluorescence quenching of HSA, which was mainly due to static quenching. The binding constant and binding site of Sal A and has been obtained in different temperatures. Analysis of thermodynamic parameters, the combination of Sal A and HSA is a spontaneous exothermic process and the force between them is hydrogen bonds and van der Waals forces.
Key words: salvianolic acid A; human serum albumin; UV-visible absorption spectroscopy; fluorescence
引用本文：朱西挺, 熊晨, 周杨, 等. 丹酚酸A与人血清白蛋白的相互作用研究[J]. 化学试剂, 2020, 42(7)：836-839 .
注射用盐酸丙帕他莫无菌检查方法适用性研究
陈扣宝*，吕小燕
（合肥市食品药品检验中心，安徽 合肥 230088）
摘要：按照2015年版《中国药典》四部通则1101中的规定，对注射用盐酸丙帕他莫进行无菌检查方法适用性研究，建立该样品的无菌检查方法。通过采用薄膜过滤法，每支样品用5 mL浓度为20 mg/mL的专用溶媒枸橼酸钠注射液溶解，再以0.1%无菌蛋白胨水溶液为冲洗液，分别冲洗200、300、400mL/筒进行试验，观察各试验组的菌生长情况。结果表明，阴性对照和样品组均无菌生长，在3d内所有阳性对照组和冲洗量400mL/筒时的试验组，菌生长良好。因此注射用盐酸丙帕他莫无菌检查，可采用薄膜过滤法，每支样品用5 mL浓度为20 mg/mL的专用溶媒枸橼酸钠注射液溶解，过滤相当于3.0 g供试品后，再以0.1%无菌蛋白胨水溶液冲洗400 mL/筒，以金黄色葡萄球菌作为阳性对照菌。
关键词: 盐酸丙帕他莫；无菌检查；方法适用性；薄膜过滤法；注射剂
中图分类号：R927.1 文献标识码：A 文章编号：0258-3283（2020）07--
Applicability of Sterility Test Method for Injection Propacetamol Hydrochloride CHEN Kou-bao*, LV Xiao-yan(Hefei Food and Drug Inspection Center, Hefei 230088, China), Huaxue Shiji, 2020, 42(7), ～
Abstract: Based on the provisions of the general rule 1101 of the fourth part of the Chinese Pharmacopoeia (2015 Edition), the applicability of the sterility test method of propacetamol hydrochloride for injection was investigated, and the sterility test method of the sample was established. By means of membrane filtration, each sample was dissolved by 5 mL of special solvent sodium citrate injection with a concentration of 20 mg/mL, and then 0.1% sterile peptone aqueous solution was used as rinse solution, each cylinder was rinsed 200 mL, 300 mL and 400 mL, respectively, and the growth of bacteria in each test group was observed. The results showed that both the negative control group and the sample group grew asepsis, and the positive control group and the test group at 400 mL per tube grew well within 3 days. Therefore, film filtration method can be adopted for propacetamol hydrochloride sterility test. Each sample is dissolved with 5 mL of 20 mg/mL of the special solvent sodium citrate injection, which is equivalent to 3.0 g of the sample, and then 400 mL of each tube is washed with 0.1% aseptic peptone solution, with staphylococcus aureus as the positive control bacteria.
Key words: propacetamol hydrochloride; sterility test; applicability of the method; membrane filtration; injection
引用本文：陈扣宝，吕小燕. 注射用盐酸丙帕他莫无菌检查方法适用性研究[J].化学试剂，2020，42(7)：840-844.
表面活性剂结构对其在水-空气界面吸附性影响
蓝艳姣a，邹梦君a，黄钦a, b, c，赵彦芝a, b，许海棠a, b, c，周菊英*a, b, c
（广西民族大学 a. 化学化工学院，b. 广西林产化学与工程重点实验室，c. 广西高校食品安全与药物分析化学重点实验室，广西 南宁 530006）
摘要：研究了聚乙二醇-马来松香-聚乙二醇三嵌段共聚物和聚乙二醇-聚丙二醇-聚乙二醇三嵌段共聚物（P123）表面活性剂在水-空气表面的吸附行为并对结构的影响进行了评价。考察了不同结构对吸附行为的影响，包括临界胶束浓度（CMC），形态转变和吸附量。利用再定向理论研究了聚氧乙烯基表面活性剂在水-空气表面的吸附和形态转变过程。随着表面活性剂浓度的增加，在水-空气表面溶剂的摩尔分数降低，表面活性剂在水-空气界面上的摩尔分数增加。计算了吸附在表面上的状态1和状态2表面活性剂的吸附量。吸附的自由能远小于胶束形成的自由能，表明表面活性剂优先吸附在表面上，达到饱和后就形成胶束。
关键词：聚氧乙烯基表面活性剂；界面；吸附行为；结构；形态转变
中图分类号：TQ423 文献标识码：A 文章编号：0258-3283（2020）
Influence of Surfactant Structure on Adsorption Properties between Water and Air on Interface LAN Yan-jiao1, ZOU Meng-jun1, HUANG Qin1, 2, 3, ZHAO Yan-zhi1, 2, XU Hai-tang1, 2, 3, ZHOU Ju-ying*1, 2, 3(a. School of Chemistry and Chemical Engineering, b. Guangxi Key Laboratory of Chemistry and Engineering of Forest Products, c. Key Laboratory of Guangxi Colleges and Universities for Food Safety and Pharmaceutical Analytical Chemistry, Guangxi University for Nationalities, Nanning 530006, China), Huaxue Shiji, 2020, 42(7)
Abstract: The influence of structural properties on the adsorption behaviors of polyoxyethylene-maleated rosin- polyoxyethylene copolymer and polyethylene-polypropylene glycol-polyethylene（P123） surfactants was evaluated. The effects of structure on adsorption behavior including critical micelle concentration (CMC), morphological change, and adsorption capacity were investigated. Reorientation theory was put forward to depict the adsorption and the morphological transformation for polyoxyethylene-based surfactants on interface between water and air. The solvent molar fraction decreased and that of surfactant molecules increased as copolymer concentration increased. The amount of state 1 and state 2 surfactants adsorbing on the surface were calculated. The free energy of adsorption is far less than the energy of micellar formation, indicating the surfactants are preferably adsorbed on the surface and shaped into micelles once saturated adsorptions are achieved. The consequences are helpful to illustrate the structure effect on adsorption behaviors and to expand in the formulation of micelles.
Key words: polyoxyethylene-based surfactant; surface; adsorption behavior; structural properties; morphological change
引用本文：蓝艳姣, 邹梦君, 黄钦, 等. 表面活性剂结构对其在水-空气界面吸附性影响[J]. 化学试剂, 2020, 42(7):845-851.
七、八元瓜环与N-苄基氨基嘌呤的自组装体系研究
李春荣*，孟铁宏，刘仕云，姜艳萍，胡先运
（黔南民族医学高等专科学校 贵州 都匀 558000）
摘要：利用紫外-可见吸收光谱、氢核磁共振技术、基质辅助激光解析电离飞行时间质谱、红外光谱、及热重分析等方法分析了七元瓜环（Q[7]）、八元瓜环（Q[8]）与N-苄基氨基嘌呤（NBAP）的主客体作用模式，并进行了自组装包结物的细胞毒性测试和细胞成像研究。实验结果表明Q[7，8]与NBAP分别以不同的作用模式自组装形成了1:1的包合物。NBAP完全进入Q[8]空腔所形成包结配合物的热稳定性强于Q[7]-NBAP配合物的稳定性。两种包结物的形成均降低了NBAP的细胞毒性，细胞成像结果进一步验证了两种包结物以不同包结模式完成了自组装。
关键词：瓜环；自组装；包结物；NBAP
中图分类号：O625.6 文献标识码：A 文章编号：0258-3283（2020）--
Self-assembly System Between Cucurbit[7，8]uril and N-benzylaminopurine LI Chun-rong*, MENG Tie-hong, LIU Shi-yun, JIANG Yan-ping, HU Xian-yun (Qiannan Medical College for Nationalities, Duyun 558000, China) Huaxue Shiji, 2020, 42(7), ～
Abstract: Host-guest interaction of cucurbit[n]urilsQ[7] and Q[8] with N-benzylaminopurine (NBAP) were investigated by using UV-vis absorbance, 1HNMR, MALDI-TOF, IR and TGA methods. The result indicated that 1:1 inclusion complex of Q[7,8] with NBAP were formed by different self-assembly model. The cytotoxicity and imaging of self-assembly inclusion complex in cells were verified. Thermal stability of inclusion complex Q[8]-NBAP stronger than that of Q[7]-NBAP complex. The formation of inclusion complex reduced the cytotoxicity of NBAP, furthermore, the different self-assembling models of the inclusion complex were confirmed by using cell images.
Key words: Cucurbit[n]urils; self-assembly; inclusion complex；NBAP
引用本文：李春荣，孟铁宏，刘仕云，等. 七、八元瓜环与N-苄基氨基嘌呤的自组装体系研究[J]. 化学试剂, 2020, 42(7): 852-857.
细辛脑中蓝色荧光杂质生成机理与结构鉴定
王冠蕾，刘涛，马丽，侯士法*
（承德石油高等专科学校 化学工程系，河北 承德 067000）
摘要：细辛脑原料药中含有一种有害的蓝色荧光杂质且难以去除，但关于其生成机理、分子结构、性质等相关研究尚未见报道。本研究采用气相色谱法考察了α-细辛脑在不同溶剂中的蓝色荧光杂质含量的变化，探讨了蓝色荧光杂质生成条件和机理，合成了蓝色荧光杂质并通过核磁、红外光谱、质谱鉴定了其分子结构。结果表明：蓝色荧光杂质是2,4,5-三甲氧基苯甲醛，由空气氧化细辛脑生成，酸性介质具有催化作用。以细辛脑为原料，高碘酸钠水溶液作氧化剂，在乙酸-甲醇介质中合成了蓝色荧光杂质，收率为5.9%，熔点为111～113℃。
关键词：细辛脑；结构鉴定；蓝色荧光杂质；2,4,5-三甲氧基苯甲醛；合成
中图分类号：O656.4 文献标识码：A 文章编号：0258-3283(2020)
Formation Mechanism and Structure Identification of Blue Fluorescent Impurity in Asarone
WANG Guan-lei, LIU Tao, MA Li, HOU Shi-fa*(Department of Chemical Engineering, Chengde Petroleum College, Chengde 067000, China), HuaxueShiji, 2020, 42(7)
Abstract: A harmful impurity of blue fluorescence is present in the raw asarone drug and difficult to remove. However, the research on its formation mechanism, formula structure and properties has not yet reported. Gas chromatography was applied to investigate the change of blue fluorescent impurity content of α-asarone in different solvents. The formation conditions and mechanism of blue fluorescent impurities were investigated. The blue fluorescent impurity was synthesized and its molecular structure was confirmed by NMR, IR and MS. The blue fluorescent impurity is 2,4,5-trimethoxybenzaldehyde, which is formed from the oxidation of asarone by air, acid medium has catalytic effect on the oxidation of asarone. The fluorescent impurity was synthesized from asarone and sodium periodate aqueous solution as oxidant in acid medium, yield was 5.9%, and the melting point was 111～ 113℃.
Key words: asarone; structure identification; blue fluorescent impurity; 2,4,5-trimethoxy-benzaldehyde; synthesis
引用本文：王冠蕾，刘涛，马丽，等. 细辛脑中蓝色荧光杂质生成机理与结构鉴定[J].化学试剂，2020，42(7)：858-861.
咪唑类离子液体在蒜素提取中的应用
贾晓丽, 王鑫, 赵三虎*
(忻州师范学院 化学系, 山西 忻州 034000)
摘要：合成系列咪唑类离子液体并作为溶剂用于新鲜大蒜中蒜素的提取。通过单因素试验和正交试验，比较了离子液体烷基链、料液比、离子液体浓度、超声时间等因素对提取效率的影响，发现影响蒜素提取率的各因素之间的关系为：料液比>酶解温度>乙醇体积分数>离子液体浓度>超声时间。由正交实验优选得：[C2mim]Br浓度为0.8 mol/L（90%乙醇溶解），料液比为1:4（g/mL），酶解温度为30 ℃，酶解时间为45 min，超声时间为40 min，超声功率为80 W，超声温度为30 ℃时，提取率最高，达0.4216%。
关键词：大蒜素；离子液体；分光光度法；超声；提取
中图分类号： O628.2 文献标识码：A 文章编号：0258-3283(2020)
Application of Imidazonium Ionic Liquids in the Extraction of Allicin JIA Xiao-li, WANG Xin, ZHAO San-hu (Department of Chemistry, Xinzhou Teachers University, Xinzhou 034000, China), Huaxue Shiji, 2020, 42(7)
Abstract: A series of imidazonium ionic liquids were synthesized and used as solvents in the extraction of allicin from fresh garlic. The single factor test and orthogonal test showed that the main factor affecting the extraction rate and the relationship between the influencing factors is as follows: material-liquid ratio>enzymatic temperature>ethanol volume fraction>ionic liquid concentration>ultrasonic time. Further optimization by orthogonal experiment showed that the extraction rate is 0.4216% when the extractant is 0.8 mol/L [C2mim]Br(with 90% ethanol as solvent), the solid-liquid ratio is 1:4 , the enzymolysis temperature is 30 ℃, the enzymolysis time is 45 minutes, the ultrasonic temperature is 30 ℃, the ultrasonic power is 80 W and the ultrasonic time is 40 minutes.
Key words: allicin; ionic liquid; spectrophotometry; ultrasound; extract
引用本文：贾晓丽, 王鑫, 赵三虎. 咪唑类离子液体在蒜素提取中的应用[J].化学试剂，2020，42（7）:862-867.
响应面法优化超声辅助提取土壤中的有效态铅镉锌镍铜
熊文明1，谢彩玲1，李拥军*2，莫桂民1，韦秀胆3
（1.中山火炬职业技术学院，广东 中山 528436；2. 清远职业技术学院，广东 清远 511510；3.广东利诚检测技术有限公司，广东 中山 528436）
摘要：建立了响应面法-超声辅助提取土壤中5种有效态重金属的方法。试验在单因素基础上，根据Box-Behnken中心组合试验设计，采用三因素三水平数学模型和响应面法，考察各个因素对土壤中有效态重金属提取效果的影响。结果表明：有效态重金属超声辅助提取的最佳条件为：超声时间30 min；提取功率252 W；提取液pH 7.3。在选定的条件下有效态重金属提取率与环境部标准方法基本一致，且提取时间缩短至30 min。响应面法优化得到的提取条件操作易得，可作为土壤中有效态重金属提取的一种有效方法。
关键词：响应面法；超声提取；土壤；有效态重金属；Box-Behnken设计
中图分类号：X833 文献标识码：A 文章编号：0258-3283（2020）
Ultrasonic Assisted Extraction of Lead, Cadmium, Zinc, Nickel and Copper from Soil by Response Surface Method XIONG Wen-ming1, XIE Cai-ling1, LI Yong-jun*2,MO Gui-min1,WEI Xiu-Dan3(1.Zhongshan Torch Polytechnic, Zhongshan 528436, China；2.Qinyuan Polytechnic, Qinyuan 511510, China；3.Guangdong Licheng Detection Technology Co., Ltd，Zhongshan 528436, China), Huaxue Shiji, 2020, 42(7)
Abstract：A response surface method-ultrasonic assisted extraction of five available heavy metals from soil was established. Based on the design of Box-Behnken central combination experiment, the effects of each factor on the effective extraction of heavy metals in soil were investigated by using three factors and three level mathematical model and response surface method. The results showed that the optimum conditions of ultrasonic assisted extraction of available heavy metals were as follows: ultrasonic time 30 min, extraction power 252W, and pH 7.3. Under the selected conditions, the effective extraction rate of heavy metals is basically consistent with the standard method of the ministry of environment, and the extraction time is shortened to half an hour. The extraction conditions optimized by response surface method are easy to be obtained and can be used as an effective method for the extraction of available heavy metals in soil.
Key words：response surface method; ultrasonic assisted extraction ;soil; available heavy metals
引用本文：熊文明，谢彩玲，李拥军，等.响应面法优化超声辅助提取土壤中的有效态铅镉锌镍铜[J].化学试剂，2020，42（7）:868-873.
新型阿利苯醇衍生物的合成及表征
李海峰1，欧阳红霞*2，陈志军1，吕巧莉1
（1. 江西省肿瘤医院核医学科 江西省肿瘤转化医学重点实验室，江西 南昌 330029；2. 南昌大学抚州医学院，江西 抚州 344000)
摘要：以阿利苯醇为先导化合物，对其结构进行分析、修饰，以邻香兰素为起始原料，经醚化、氧化、酰氯化、酰胺化等反应合成了5种新型Alibendol衍生物。并对目标产物合成的物质的量比、合成方法等反应条件进行优化。所有目标产物、中间体化合物通过IR、1H NMR等对其结构进行了表征确认。
关键词：酰胺化；合成；表征； 阿利苯醇；衍生物
中图分类号：O621.256.4 文献标识码：A 文章编号：0258-3283（2020）
Synthesis and Characterization of Novel Alibendol Derivatives LI Hai-feng1, OUYANG Hong-xia*2, CHEN Zhi-jun1, LV Qiao-li1 (1. Depatment of Nuclear Medicine, Jiangxi Cancer Hospital, Department of Jiangxi Key Laboratory of Translationl Cancer Research, Nanchang 330029, China; 2. Fuzhou Medical College of Nanchang University, Fuzhou 344000, China), Huaxue Shiji, 2020, 42(7)
Abstract: The structure of the lead compound of alibendol was analyzed and modified, five novel alibendol derivatives were designed and synthesized via a sequence of etherification, oxidation, acyl chloridization, amidation, etc. Five kinds of novel alibendol derivatives were synthesized using 3-methoxysalicylaldehyde as raw material. The reaction conditions of the mole ratio of reactants, synthetic methods were optimized and the structures of intermediates and the targets were confirmed by 1HNMR and IR etc.
Key words: amidation; synthesis; characterization; alibendol; derivative
引用本文：李海峰, 欧阳红霞, 陈志军, 等. 新型阿利苯醇衍生物的合成及表征[J]. 化学试剂, 2020, 42(7):874-878.
含两个2,2’-二联吡啶芳香羧酸的合成与表征
万屏南，樊燕，肖文杰，于玲玲，林艳*，崔汉峰*
(江西中医药大学 药学院，江西 南昌 330004)
摘要：以廉价易得的2-乙酰基吡啶为起始原料，经2-吡啶酰基碘化吡啶合成中间体5-甲基-2,2’-二联吡啶，再经溴代、烷基化、水解反应，设计合成了含两个2,2’-二联吡啶芳基羧酸。目标产物的结构经1HNMR、13CNMR和HRMS进行确证。重点考察了溴代反应的最佳工艺条件，结果表明5-甲基-2,2’-二联吡啶与NBS的物质的量比为1：1.1，反应时间10 h，温度为60 ℃条件下能以较高产率获得一溴代产物。
关键词：二联吡啶；芳香羧酸；合成；表征；溴代反应
中图分类号：O625.64 文献标识码：A 文章编号：0258-3283（2020）
Synthesis and Characterization of Aromatic Carboxylic Acid Containing Two 2,2'- Bipyridines WAN Ping-nan, FAN yan, XIAO Wen-jie, YU Ling-ling, LIN Yan*, CUI Han-feng* (School of Pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China), Huaxue Shiji, 2020, 42(7)
Abstract：A novel aromatic carboxylic acid containing two 2,2'- bipyridines was designed and synthesized by bromination, alkylation and hydrolysis reaction with intermediate 5-methyl-2,2'- bipyridine which obtained from 2-acetylpyridine as a starting material. The starting material is very cheap and easy to be obtained. The structures of the target product and intermediates were confirmed by 1HNMR, 13CNMR and HRMS. The optimized reaction conditions were obtained by screening the conditions of brominated reaction. The results showed that the molar ratio of 5-methyl-2,2'- bipyridine to NBS was 1:1.1, the reaction time was 10 h, and the yield of brominated product was higher at 60℃.
Key words：2,2'- bipyridines; aromatic carboxylic acid; synthesis; characterization；bromination reaction
引用本文：万屏南，樊燕，肖文杰，等. 含两个2,2’-二联吡啶芳香羧酸的合成与表征[J].化学试剂，2020，42（7）:879-882.
(S)-2-[羟基(二苯基)甲基]-1-甲基吡咯烷(DPMPM)的合成
毛远湖1,2，汤磊2，吴熔鑫1，吴强1，程飞1，彭鸿曼3，张吉泉*1,2
（1. 贵州医科大学 药学院, 贵州 贵阳 550004; 2.贵州省化学合成药物研发利用工程技术研究中心，贵州 贵阳 550004; 3. 贵州省贵阳市妇幼保健院，贵州 贵阳 550003）
摘要：对标题化合物的合成方法进行了改进。以L-脯氨酸为起始原料，与甲醛在Zn/NaH2PO4条件下发生还原氨化反应得中间体N-甲基-L-脯氨酸，再经乙酯化得N-甲基-L-脯氨酸乙酯，最后与苯基溴化镁发生格氏反应得标题化合物，总收率51.3％，纯度>97%。该路线操作简便、反应温和，可用于标题化合物的放大合成。
关键词：(S)-2-[羟基(二苯基)甲基]-1-甲基吡咯烷；DPMPM；手性辅助试剂；格氏反应；合成
中图分类号：R914 文献标识码：A 文章编号：0258-3283（2020）
Synthesis of (S)-2-[Hydroxy(diphenyl)methyl]-1-methylpyrrolidine MAO Yuan-hu1,2, TANG Lei2, WU Rong-xin1, WU Qiang1, CHENG Fei1, PENG Hong-man3, ZHANG Ji-quan*1,2 (1.College of Pharmacy, Guizhou Medical University, Guiyang 550004,China; 2. Guizhou Provincial Engineering Technology Research Center for Chemical Drug R&D, Guiyang 550004,China; 3.Guiyang Municipal Maternal and Child Health Care Hospital , Guiyang 550003,China), Huaxue Shiji, 2020, 42(7)
Abstract: This work reported the improved synthesis of (S)-2-[hydroxyl(diphenyl)methyl]-1-methylpyrrolidine. Starting from L-proline, the intermediate N-methyl-L-proline was obtained via reductive amination using Zn/NaH2PO4, which underwent acetylation to give intermediate. The title compound was finally prepared from 4 and phenylmagnesium bromide under Grignard reaction in an overall yield of 51.3% and a purity of more than 97%. This procedure was characterized by handy operations and mild conditions and thus, it was suitable for the scale-up preparation of the title compound .
Key words:(S)-2-[hydroxy(diphenyl)methyl]-1-methylpyrrolidine; DPMPM; chiral auxiliary reagent; Grignard reaction; synthesis
引用本文：毛远湖，汤磊，吴熔鑫，等. (S)-2-[羟基(二苯基)甲基]-1-甲基吡咯烷(DPMPM)的合成[J]. 化学试剂，2020，42（7）:883-886.
