摘要
目的:建立顶空气相色谱法,同时考察药用复合硬片中偏二氯乙烯、1,1-二氯乙烷和1,2-二氯乙烷的残留量。方法:炉温80℃,顶空平衡时间20 min,进样口温度220℃,分流比10∶1;采用DB-624石英毛细管柱(30 m×0.32 mm,1.8μm),载气为高纯氮气(纯度99.999%),流量1.0 mL·min^(-1),柱温为程序升温(35℃保持8 min,以20℃·min^(-1)升至70℃保持3 min,再以100℃·min^(-1)升至220℃保持5 min),FID检测器温度250℃。结果:偏二氯乙烯、1,1-二氯乙烷和1,2-二氯乙烷进样量分别在0.06~4μg、0.015~6μg、0.006~2.4μg范围内线性关系良好,相关系数r依次为0.9968、0.9991、0.9994;三者的加标回收率分别为104.2%、102.2%、96.2%,精密度依次为3.4%、5.2%、4.5%。结论:本方法操作简单,结果准确,灵敏度高,重复性较好,可用于药用复合硬片中偏二氯乙烯、1,1-二氯乙烷和1,2-二氯乙烷残留量的测定。
Objective:To establish a headspace gas chromatography method that can simultaneously determine the residues of vinylidene chloride,1,1-dichloroethane and 1,2-dichloroethane in medicinal composite hard tablets.Methods:Equilibrate the headspace vial at 80℃,for 20 min.The sample inlet temperature was 220℃,and the split ratio was 10∶1.DB-624 column(30 m×0.32 mm,1.8μm)was used with high-purity nitrogen(purity 99.999%)as the carrier gas.The flow rate was 1.0 mL·min^(-1).The column temperature was maintained at 35℃for 8 min,increased to 70℃at 20℃·min^(-1)for 3 min,and then increased to 220℃at 100℃·min^(-1)for 5 min.The FID detector temperature was 250℃.Results:The linear ranges of vinylidene chloride,1,1-dichloroethane and 1,2-dichloroethane were 0.06-4μg(r=0.9968)、0.015-6μg(r=0.9991)and 0.006-2.4μg(r=0.9994),respectively.The recoveries were 104.2%,102.2%and 96.2%respectively,and the precisions were 3.4%,5.2%and 4.5%respectively.Conclusion:The method is simple,accurate,sensitive and reproducible.It can be used for the determination of vinylidene chloride,1,1-dichloroethane and1,2-dichloroethane residues in medicinal composite hard tablets.
作者
冯雨薇
吴红洋
曹汐
范能全
FENG Yu-wei;WU Hong-yang;CAO Xi;FAN Neng-quan(Chongqing Institute for Food and Drug Control,Chongqing 401121,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第12期2163-2168,共6页
Chinese Journal of Pharmaceutical Analysis
作者简介
第一作者:冯雨薇,Tel:(023)86072759,E-mail:646582438@qq.com;通信作者:范能全,Tel:(023)86067359,E-mail:fannqcq@163.com。
