衍生化-顶空气相色谱法测定环丙沙星及其盐酸盐中痕量基因毒性杂质硫酸二甲酯

潘芳芳; 徐东海; 邵鹏; 汪佳楠; 郑金琪

doi:10.13748/j.cnki.issn1007-7693.20232621

衍生化-顶空气相色谱法测定环丙沙星及其盐酸盐中痕量基因毒性杂质硫酸二甲酯

Ultra Trace-level Determination of Genotoxic Impurity Dimethyl Sulfate in Ciprofloxacin and Its Hydrochloride by Derivation-headspace Gas Chromatography Method

摘要

摘要:
目的建立衍生化-顶空气相色谱法测定环丙沙星及其盐酸盐中痕量基因毒性杂质硫酸二甲酯的残留量。
方法以碘化钠为衍生化试剂，使硫酸二甲酯发生烷基化反应生成碘甲烷，通过测定碘甲烷计算硫酸二甲酯的含量；采用DB-Wax毛细管柱(30 m×0.53 mm，1.0 μm)，程序升温，初始温度为 60 ℃，维持2 min，以40 ℃·min⁻¹升到180 ℃，维持2 min；以氮气为载气，流速为3.0 mL·min⁻¹，检测器为电子捕获检测器(electron capture detector，ECD)。
结果空白试验基本无干扰；硫酸二甲酯在8.50~63.76 ng·mL⁻¹内线性关系良好(r=0.9969)；定量限浓度为2.1×10⁻⁹ g·mL⁻¹；环丙沙星和盐酸环丙沙星中硫酸二甲酯的加样回收率分别为89.3%和86.6%(n=9)。测得6批样品硫酸二甲酯残留量均小于定量限。
结论该方法操作简便、准确度高、灵敏度高、耐用性好，可用于检测环丙沙星及其盐酸盐中痕量级硫酸二甲酯的残留量。

Abstract:
OBJECTIVE To establish a derivation-headspace gas chromatography method for the determination of ultra trace genotoxic impurity dimethyl sulfate in ciprofloxacin and its hydrochloride.
METHODS Using sodium iodide as derivatization reagent, dimethyl sulfate was alkylated to produce iodomethane. The content of dimethyl sulfate was calculated by measuring iodomethane. Column was DB-Wax(30 m×0.53 mm, 1.0 μm), carrier gas was nitrogen. The flow rate was 3.0 mL·min⁻¹. The detector was electron capture detector(ECD). The initial temperature was 60 ℃, hold 2 min, then the temperature was raised to 180 ℃ at 40 ℃·min⁻¹, hold 2 min.
RESULTS There was no interference in the blank test. The linear relationship of dimethyl sulfate in the range of 8.50−63.76 ng·mL⁻¹ was good(r=0.9969), the LOQ was 2.1×10⁻⁹ g·mL⁻¹. The average recovery were 89.3% and 86.6%(n=9) in ciprofloxacin and ciprofloxacin hydrochloride. The residues of dimethyl sulfate in 6 batches of samples were all lower than the LOQ.
CONCLUSION The established method is simple, accurate, sensitive and durable for limit test and quantitative analysis of dimethyl sulfate in ciprofloxacin and its hydrochloride.

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