溴化丁基橡胶垫片中硫单质的测定及其向药物中迁移研究

Determination of Sulfur in Brominated Butyl Rubber Gasket and Its Migrating Research to Drugs

目的建立HPLC测定溴化丁基橡胶垫片中硫单质的方法,并对其向清心安神口服液迁移进行研究。方法采用Dikma Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm);检测波长为272 nm;流动相为乙腈-四氢呋喃-水(60∶30∶10);柱温为30℃;流速为1.0 mL·min^(-1)。结果硫单质在0.023~233.228μg·mL^(-1)内线性关系良好(r=0.9999),定量限为0.02332μg·mL^(-1),检出限为0.005831μg·mL^(-1),加样回收率为93.4%,迁移回收率为95.6%。结论方法简便快速、准确可靠、重复性好,可用于溴化丁基橡胶垫片中硫单质的测定,为国家药典增订硫单质的测定提供实验基础。

OBJECTIVE To establish a method for the determination of sulfur in brominated butyl rubber gasket and its migrating research to Qingxin’anshen oral liquid by HPLC.METHODS The Dikma Diamonsil C_(18) column(250 mm×4.6 mm,5μm)was used with the mobile phase of acetonitrile-tetrahydrofuran-water(60∶30∶10).The wavelength was 272 nm.The column temperature was 30℃.The flow rate was 1.0 mL·min^(-1).RESULTS The calibration curve of sulfur was linear over the range of 0.023−233.228μg·mL^(-1)(r=0.9999).The limit of quantification was 0.02332μg·mL^(-1).The detection limit was 0.005831μg·mL^(-1).The sample recovery rate was 93.4%,and the migration recovery rate was 95.6%.CONCLUSION The method is simple,rapid,accurate,reliable and reproducible.It can be used for the determination of elemental sulfur in brominated butyl rubber gaskets,and provides an experimental basis for the determination of elemental sulfur in the national pharmacopoeia.