高效液相色谱法测定药用胶塞中的二甲基二硫代氨基甲酸锌  

Determination of zinc dimethyldithiocarbamate in pharmaceutical rubber closures by high performance liquid chromatography

作　　者：谢兰桂[1] 袁淑胜 韩小旭 杨会英[1] 赵霞[1] 肖新月[1] XIE Langui;YUAN Shusheng;HAN Xiaoxu;YANG Huiying;ZHAO Xia;XIAO Xinyue(National Institutes for Food and Drug Control NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing,100050,China)

机构地区：[1]中国食品药品检定研究院药用辅料质量研究与评价重点实验室,北京100050

出　　处：《环境化学》2021年第11期3631-3634,共4页Environmental Chemistry

摘　　要：建立高效液相色谱法测定药用胶塞中二甲基二硫代氨基甲酸锌残留量.药用胶塞粉碎后经20%氨水超声提取,以含0.02 mol·L^(-1)四丁基硫酸铵的20%氨水溶液-乙腈(20:80)为流动相,经亲水性聚合物色谱柱(300 mm×7.8 mm, 5μm)分离后,254 nm波长检测.方法学结果显示二甲基二硫代氨基甲酸锌在100—750μg·mL^(-1)质量浓度范围内线性良好,相关系数为0.9991,检出限和定量限分别为1.6 ng和2.5 ng,高、中、低溶液精密度RSD小于0.7%,溶液在12 h内稳定,加标回收率为99.9%-101.5%.实际药用胶塞检测,样品中未检出二甲基二硫代氨基甲酸锌.方法简便、稳定,适用于测定药用胶塞中二甲基二硫代氨基甲酸锌残留.To establish a HPLC method for the determination of zinc dimethyldithiocarbamate residues in pharmaceutical rubber closures. The pharmaceutical rubber closures were crushed and ultrasonically extracted with 20% ammonia water. The mixed solution of ammonia water and acetonitrile(20:80)(containing 0.02 mol·L^(-1) tetra butyl ammonium sulfate) was used as the mobile phase, a hydrophilic polymer chromatographic column(300 mm×7.8 mm, 5 μm) was used as the chromatographic column, and the detection wavelength was 254 nm. No zinc dimethyldithiocarbamate was detected in the medicinal stopper. The methodological results showed that the linear range of zinc dimethyldithiocarbamate was 100-750 g·mL^(-1), the correlation coefficient was 0.9991, and the detection limit and quantitative limit were 1.6 ng and 2.5 ng respectively. The precision(expressed by RSD) of high, medium, and low concentration solution was less than 0.7%, the solution was stable within 12 hours, and the recovery rate of standard addition was 99.9% to 101.5%. The method in this study was simple, stable, and suitable for the determination of zinc dimethyldithiocarbamate residues in pharmaceutical rubber closures.

关 键 词：药用胶塞 二甲基二硫代氨基甲酸锌 高效液相色谱法 硫化促进剂 金属螯合物 

分 类 号：O657.72[理学—分析化学] TQ460.69[理学—化学]