药用胶塞中二丁基二硫代氨基甲酸锌的高效液相色谱分析方法研究  

Study on HPLC Analysis of Zinc Dibutyldithiocarbamate in Pharmaceutical Rubber Stoppers

作　　者：谢兰桂[1,2] 袁淑胜 韩小旭 杨会英 赵霞[1,2] 肖新月 XIE Langui;YUAN Shusheng;HAN Xiaoxu;YANG Huiying;ZHAO Xia;XIAO Xinyue(National Institutes for Food and Drug Control,Beijing 100050,China;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,北京100050 [2]国家药品监督管理局药用辅料质量研究与评价重点实验室,北京100050

出　　处：《橡胶工业》2022年第7期547-551,共5页China Rubber Industry

基　　金：国家药典委员会药品标准制修订研究课题(2018Y011)。

摘　　要：建立高效液相色谱(HPLC)法测定药用胶塞中二丁基二硫代氨基甲酸锌的残留量的方法。药用胶塞浸于液氮脆化后粉碎,经四氢呋喃-乙腈(体积比为10∶90)超声提取制得供试品溶液。以四氢呋喃-乙腈(体积比为35∶65)为流动相,供试品溶液经SunFire C_(18)色谱柱(4.6 mm×250 mm,5μm)分离后,用254 nm检测波长进行HPLC测试。试验结果显示:二丁基二硫代氨基甲酸锌的质量浓度在20~750μg·mL^(-1)范围内与HPLC峰面积的线性相关性良好,相关因数为0.9999;高、中、低质量浓度的供试品溶液的HPLC峰面积的相对标准偏差小于3%,测试精密度高;本方法检出限和定量限分别为20和30 ng,加标回收率为98.84~102.58%,供试品溶液在6 h内稳定。本方法简便、准确、灵敏、稳定,适用于测定药用胶塞中二丁基二硫代氨基甲酸锌的残留量。A high-performance liquid chromatography(HPLC)method was established to determine the residual amount of zinc dibutyldithiocarbamate in pharmaceutical rubber stoppers.The pharmaceutical rubber stopper was pulverized after being embrittled in liquid nitrogen,and then it was ultrasonically extracted with tetrahydrofuran-acetonitrile(volume ratio of 10∶90)to prepare a test solution.The tetrahydrofuran-acetonitrile(volume ratio of 35∶65)was used as the mobile phase,after passing through SunFire C_(18) chromatographic column(4.6 mm×250 mm,5μm)for separation,the test solution was tested by HPLC with the detection wavelength of 254 nm.The results showed that the mass concentration of zinc dibutyldithiocarbamate in 20~750μg·mL^(-1) had a good linearity correlation with the HPLC peak area,the correlation coefficient was 0.9999.The relative standard deviations of HPLC peak area of the test solutions with high,medium and low concentration were less than 3%,and the test precision was high.The detection limit and quantification limit of this test were 20 and 30 ng respectively,the recovery rate was 98.84%~102.58%,and the test solution was stable within 6 h.This method established in this paper was simple,accurate,sensitive,stable,and it was suitable for the determination of the residual amount of zinc dibutyldithiocarbamate in pharmaceutical rubber stoppers.

关 键 词：药用胶塞 二丁基二硫代氨基甲酸锌 高效液相色谱法 金属螯合物 

分 类 号：TQ336.6[化学工程—橡胶工业] TQ330.385