摘要
目的建立测定药用胶塞中正己烷含量的气相色谱法。方法采用气相色谱法测定氯化丁基胶塞中正己烷的含量及在包装药品中的迁移情况。色谱柱为DB-624毛细管柱(30 m×0.320 mm,1.80μm);FID检测器,温度为280℃;载气为N2;柱流量为2.0 mL/min;柱温采用程序升温,45℃保持7 min,8℃/min升至110℃保持7 min,60℃/min升至250℃保持3 min;进样口温度为280℃,分流比为20∶1,进样量为1μL。结果正己烷质量浓度在0.5~50μg/mL范围内与峰面积线性关系良好(R2=1),在19 h内稳定性良好,检出限为0.22μg/mL,平均加样回收率为95.75%(n=9);氯化丁基胶塞中正己烷含量为1.51μg/g,迁移药品中均未检出正己烷。结论该方法操作简单、结果准确、灵敏度高、重复性好,可用于药用胶塞中正己烷的含量测定。
Objective To establish a gas chromatography method that can determine the contents of n-hexane in medicinal rubber stopper.Methods Gas chromatography was used to determine the content of n-hexane in the chlorobutyl rubber stopper and its migration in the packaged medicines.The chromatographic column was a DB-624 capillary column(30 mm×0.320 mm,1.80μm);FID detector,t emperature 280℃;carrier gas N2,column flow rate 2.0 mL/min;the column temperature adopted the program temperature rise,kept for 7 min at 45℃,rose to 110℃at 8℃/min,kept for 7 min,rose to 250℃/min at 60℃/min,kept for 3 min;the injection temperature was 280℃,split ratio 20∶1,and the injection volume was 1μL.Results The mass concentration of n-hexane had a good linear relationship with the peak area in the range of 0.5-50μg/mL(R2=1);the stability was good within 19 h and the detection limit was 0.22μg/mL;the average recovery rate was 95.75%(n=9).The content of n-hexane in the chlorobutyl rubber plug was 1.51μg/g,and n-hexane was not detected in the migrated drugs.Conclusion The method is simple in operation,accurate in result,high in sensitivity and good in repeatability,and can be used for the determination of the content of n-hexane in medicinal rubber stoppers.
作者
吴红洋
杨大成
胡庆华
李莎
彭兰
WU Hongyang;YANG Dacheng;HU Qinghua;LI Sha;PENG Lan(Chongqing Institute for Food and Drug Control,Chongqing,China 401121;Southwest University,Chongqing,China 400715;China Medical University,Nanjing,Jiangsu,China 211198;Chongqing Medical and Pharmaceutical College,Chongqing,China 401331)
出处
《中国药业》
CAS
2020年第9期106-108,共3页
China Pharmaceuticals
基金
重庆市科研机构绩效激励引导专项项目[cstc2019jxj1130040]。
关键词
气相色谱法
药用胶塞
正己烷
迁移量
gas chromatography
medicinal rubber stopper
n-hexane
migration
