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分配系数和相比的选择在 HS-GC测定基因毒性杂质苯中的应用

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  • 1.临沂市人民医院,临沂 276003;
    2.临沂科技职业学院,临沂 276017
第一作者 Tel: 18053946527; E-mail:bxzf29@foxmail.com
* Tel:13853939786;E-mail:383854564@qq.com

修回日期: 2021-03-03

  网络出版日期: 2024-07-15

Application of partition coefficient and phase ratio selection in determining genotoxic impurity benzene by HS-GC

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  • 1. Linyi People’s Hospital,Linyi 276003,China;
    2. Linyi Vocational College of Science and Technology,Linyi 276017,China

Revised date: 2021-03-03

  Online published: 2024-07-15

摘要

目的: 建立药品中基因毒性杂质苯残留量的检测方法,为药物分析中苯的检测提供方法依据。方法: 采用 ZB-50 毛细管柱(30 m× 0.53 mm× 1.0 μm),柱温为程序升温(起始温度 40 ℃,保持 1 min,以 25 ℃· min-1 的速率升温至 180 ℃,保持 3 min);进样口 200 ℃,氢火焰离子化检测器(FID)温度为:250 ℃。载 气为氮气,流速 2.0 mL·min-1,分流比为 10∶1;顶空进样,顶空平衡温度 90 ℃,平衡时间为 20 min。结果: 苯浓度范围在 0.034~0.407 µg·mL-1 线性关系良好(r=0.999 5),平均加样回收率(n=9)为 92.3%(RSD= 2.4%),检测下限为 11.0 ng·mL-1,定量下限为 34.0 ng·mL-1,5 批样品中均未检出苯。结论: 所建立的方法能够较好地对药品中残留的苯进行限度测定,极大的提高苯的检测效率。

本文引用格式

彭纪铭, 陈娜娜, 伏瑶, 李泽, 刘文启 . 分配系数和相比的选择在 HS-GC测定基因毒性杂质苯中的应用[J]. 药物分析杂志, 2021 , 41(6) : 1029 -1035 . DOI: 10.16155/j.0254-1793.2021.06.13

Abstract

Objective: To established a method for the determination of genotoxic impurity benzene residues in drug, to provide a basis for the determination of benzene in drug analysis. Methods: A ZB-50 capillary column(30 m×0.53 mm×1.0 μm)was used,the temperature program for the column was as follows:initially heated at 40 ℃ for 1 min, increased to 180 ℃ at a speed of 25 ℃·min-1 and lasted for 3 min. The inlet temperature was 220 ℃ and FID detector -1 temperature was set at 250 ℃ . The split ratio was 10∶1 and the flow rate of the carrier gas(N2)was 2.0 mL·min . Headspace conditions were as follows:the temperature and the time of shaking for the sample were 90 ℃ and 20 min. Results: Benzene had a good linear relationship within the concentration range of 0.034-0.407 µg·mL-1r=0.999 5). The average recoveries(n=9)were 92.3%(RSD=2.4%). The limit of detection was 11.0 ng·mL-1 and the limit of quantification was 34.0 ng·mL-1. Benzene was not detected in the 5 batches of samples. Conclusion: The established method greatly improved the detection efficiency of benzene residues in pharmaceuticals.

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