药用橡胶塞中可提取硫和4-叔辛基苯酚及2-巯基苯并噻唑的检测OA北大核心CSTPCD
Simultaneous Determination of Extractable Sulfur,4-Octylphenol and 2-Nercaptobenzo-thiazole in Pharmaceutical Halogenated Butyl Rubber Stopper
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-C18(150 mm×4.6 mm,5 μm)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 20 μL.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 0.20～501.00 μg·mL-1(r=0.999 8)、0.20～502.95 μg·mL-1(r= 0.999 9)、0.22～547.53 μg·mL-1(r=0.999 8),检出限分别为 0.40、0.25 和 0.15 μg·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-octylphe-nol and 2-MBT was developed.The detection was performed on Agilent ZORBAX SB-C18 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 20 μL.Results The linear ranges of sulfur,4-octylphenol and 2-MBT were 0.20-501.00 μg·mL-1(r=0.999 8),0.20-502.95 μg·mL-1(r=0.999 9),0.22-547.53 μg·mL-1(r=0.999 8),respectively.The limits of quantitation were 0.40 μg·mL-1,0.25 μg·mL-1 and 0.15 μg·mL-1,relative standard deviations(RSDs)of pre-cision,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%,respec-tively.Conclusion The method is sensitive,rapid,convenient and reproducible,and can be used for simultaneous determina-tion of extractable sulfur,4-octylphenol and 2-MBT in pharmaceutical halogenated butyl rubber stopper.
程佳美;贾菲菲;李颖;赵霞;杨会英
中国食品药品检定研究院包装材料室,北京 100050
药学
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 stopperExtractable sulfur4-Octylphenol2-Nercaptobenzothia-zoleContent determination
《医药导报》 2024 (005)
712-716 / 5
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).
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