高效液相色谱-串联质谱法检测泮托拉唑钠原料药中的水合肼  

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

作　　者：赵会明 张振洋 樊华军 ZHAO Huiming;ZHANG Zhenyang;FAN Huajun(ICAS Testing Technology Service(Shanghai)CO.,LTD.,Shanghai 201100,China)

机构地区：[1]英格尔检测技术服务(上海)有限公司,上海201100

出　　处：《上海医药》2022年第11期72-75,共4页Shanghai Medical & Pharmaceutical Journal

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=0.9999),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。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 0.23,0.47 ng/mL and hydrazine hydrate showed good linear relationship in the range of 0.47-9.37 ng/mL(r=0.9999).The recoveries of samples at low,medium and high-level concentrations reached 81.6%to 90.9%in the accuracy experiment.No hydrazine hydrate was detected in 3 batches of pantoprazole sodium.

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 

分 类 号：R917[医药卫生—药物分析学] O657[医药卫生—药学]