摘要
目的建立药品中环氧氯丙烷有机残留大体积进样、程序升温汽化、气相色谱测定方法。方法取一定量的样品,加入二硫化碳溶液提取后大体积进样(30μL),经程序升温汽化进样-气相色谱测定,进行定量测定。结果此方法检出限0.000 15%,日内精密度6.28%~7.81%之间,日间精密度7.97%~8.94%之间,回收率89.3%~96.7%,线性范围0.145~2.360μg/mL,相关系数0.997 5。结论此法操作简单、灵敏度高,可用于测定药品中残留的环氧氯丙烷。
Objective To establish a PTV-GC(programmed temperature vaporization-gas chromatography) method for the determination of residual epichlorohydrin in drugs.Methods Epichlorohydrin in drug was extracted by carbon disulfide.The extract was analyzed by GC equipped with a programmable temperature vaporizer in large volume injection(30 μL).Results The range of calibration curve was 0.145-2.360 ug/mL(r = 0.997 5) with the detection limit of 0.000 15 %.The recovery of the method was between 89.3 % and 96.7 %.The inter-day and intra-day precision was 6.28 %-7.81 % and 7.97 %-8.94 %,respectively.Conclusion The method developed is easy to operate and with high sensitivity,so it is suitable for the determination of residual epichlorohydrin in drugs.
出处
《食品与药品》
CAS
2010年第9期335-337,共3页
Food and Drug