文章摘要
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
投稿时间：2021-11-12  修订日期：2021-11-12
DOI：10.12136/j.issn.1000-890X.2022.07.0547
中文关键词: 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
英文关键词: pharmaceutical rubber stopper  zinc dibutyldithiocarbamate  HPLC  metal chelates
基金项目:
作者单位E-mail
谢兰桂* 中国食品药品检定研究院；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 pharm215@126.com 
袁淑胜 中国食品药品检定研究院；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  
韩小旭 中国食品药品检定研究院；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  
杨会英 中国食品药品检定研究院；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  
赵　霞 中国食品药品检定研究院；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  
肖新月 中国食品药品检定研究院；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  
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中文摘要:
      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 C18色谱柱（4.6 mm×250 mm，5 μm）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20～750 μg·mL-1范围内与HPLC峰面积的线性良好，相关因数为0.999 9；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。
英文摘要:
      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 C18 chromatographic column（4. 6 mm×250 mm， 5 μm） 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 20～750 μg·mL-1 had a good linearity correlation with the HPLC peak area，the correlation coefficient was 0. 999 9.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.
Author NameAffiliationE-mail
XIE Langui National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients pharm215@126.com 
YUAN Shusheng National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients  
HAN Xiaoxu National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients  
YANG Huiying National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients  
ZHAO　Xia National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients  
XIAO Xinyue National Institutes for Food and Drug Control；NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients  
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