赵会明 张振洋 樊华军

    摘 要 建立了泮托拉唑钠原料药中的基因毒性杂质水合肼的高效液相色谱-串联质谱(LC-MSMS)检测方法。采用反相色谱，以水-乙腈(含0.1%甲酸)为流动相，梯度洗脱，流速0.5 mL/min，以ESI正离子多反应监测(MRM)模式进行质谱检测。结果显示，水合肼的检测限和定量限可达到0.23、0.47 ng/mL，其在0.47～9.37 ng/mL浓度范围内线性关系良好(r=0.999 9)，准确度试验中低、中、高浓度回收率均在81.6%～90.9%之间。在3批次泮托拉唑钠原料药中均未检出水合肼。

    关键词 高效液相色谱-串联质谱法 基因毒性杂质 泮托拉唑钠 水合肼 痕量检测

    中图分类号：R917； O657 文献标志码：A 文章编号：1006-1533(2022)11-0072-04

    引用本文 赵会明， 张振洋， 樊华军. 高效液相色谱-串联质谱法检测泮托拉唑鈉原料药中的水合肼[J]. 上海医药， 2022， 43(11)： 72-75.

    Determination of hydrazine hydrate in pantoprazole sodium by high performance liquid chromatography-tandem mass spectrometry

    ZHAO Huiming， ZHANG Zhenyang， FAN Huajun

    [ICAS Testing Technology Service (Shanghai) CO.， LTD.， Shanghai 201100， China]

    ABSTRACT To establish a high-performance liquid chromatography-tandem mass spectrometry (LC-MSMS) method for the determination of hydrazine hydrate in active pharmaceutical ingredient ( API) pantoprazole sodium. HPLC was carried out by reverse chromatography using water-acetonitrile containing 0.1% formic acid as flow phase and gradient elution at a flow rate of 0.5 mL/min. Mass spectrometry was performed with multi-reaction monitoring (MRM) in positive ESI mode. The detection and quantitative limits of hydrazine hydrate reached 0.23 ......