摘要
目的建立高效液相色谱法同时测定药用卤化丁基橡胶塞中可提取硫、4-叔辛基苯酚及2-巯基苯并噻唑的含量。方法使用甲苯-甲醇混合溶液作为提取溶剂,采用ZORBAX SB-C_(18)(150 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-水(85:15),流速1.0 mL·min^(-1),检测波长280 nm,柱温为40℃,进样量20μL。结果可提取硫、4-叔辛基苯酚和2-巯基苯并噻唑的检测质量浓度线性范围分别为0.20~501.00μg·mL^(-1)(r=0.9998)、0.20~502.95μg·mL^(-1)(r=0.9999)、0.22~547.53μg·mL^(-1)(r=0.9998),检出限分别为0.40、0.25和0.15μg·mL^(-1);精密度、稳定性的相对标准偏差(RSD)均<3%;提取回收率分别为93.5%~104.8%、99.0%~100.6%和103.0%~107.7%;迁移回收率分别为97.0%~101.8%、98.7%~110.3%和89.3%~94.0%。结论该方法灵敏快速、操作简便、重复性好,可用于药用卤化丁基橡胶塞中可提取硫、4-叔辛基苯酚及2-巯基苯并噻唑含量的测定。
Objective To establish a method for simultaneous determination of extractable sulfur,4-octylphenol and 2-nercaptobenzothiazole(2-MBT)in pharmaceutical halogenated butyl rubber stopper by HPLC.Methods The mixed solution of toluene and methanol was adopted as the extraction solvent,and a HPLC method for detection of extractable sulfur,4-octylphenol and 2-MBT was developed.The detection was performed on Agilent ZORBAX SB-C 18 column with mobile phase consisted of acetonitrile-water(85:15)at the flow rate of 1.0 mL·min^(-1).The column temperature was 40℃,and detection wavelength was set at 280 nm.The injection sample volume was 20μL.Results The linear ranges of sulfur,4-octylphenol and 2-MBT were 0.20-501.00μg·mL^(-1)(r=0.9998),0.20-502.95μg·mL^(-1)(r=0.9999),0.22-547.53μg·mL^(-1)(r=0.9998),respectively.The limits of quantitation were 0.40μg·mL^(-1),0.25μg·mL^(-1) and 0.15μg·mL^(-1),relative standard deviations(RSDs)of precision,stability and reproducibility tests were all lower than 3%.The extraction recoveries were 93.5%-104.8%,99.0%-100.6%and 103.0%-107.7%,respectively.The migration recoveries were 97.0%-101.8%,98.7%-110.3%and 89.3%-94.0%,respectively.Conclusion The method is sensitive,rapid,convenient and reproducible,and can be used for simultaneous determination of extractable sulfur,4-octylphenol and 2-MBT in pharmaceutical halogenated butyl rubber stopper.
作者
程佳美
贾菲菲
李颖
赵霞
杨会英
CHENG Jiamei;JIA Feifei;LI Ying;ZHAO Xia;YANG Huiying(Department of Packaging Materials,National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《医药导报》
CAS
北大核心
2024年第5期712-716,共5页
Herald of Medicine
基金
中国食品药品检定研究院中青年发展研究基金资助项目(2023C10)。
关键词
药用卤化丁基橡胶塞
可提取硫
4-叔辛基苯酚
2-巯基苯并噻唑
含量测定
Pharmaceutical halogenated butyl rubber stopper
Extractable sulfur
4-Octylphenol
2-Nercaptobenzothiazole
Content determination
