高效液相色谱-三重四极杆串联质谱法测定一次性静脉留置针中双酚A残留量  

Determination of Bisphenol A Residue in Intravenous Indwelling Needles by HPLC-MS/MS

作　　者：刘慧 王健 李奇 王紫芸 苟彦彦 许静远 徐力 LIU Hui;WANG Jian;LI Qi;WANG Ziyun;GOU Yanyan;XU Jingyuan;XU Li(Yangzhou Center for Food and Drug Control,Yangzhou,Jiangsu,China 225000;School of Biology and Food Engineering,Changshu Institute of Technology,Suzhou,Jiangsu,China 215500)

机构地区：[1]江苏省扬州市食品药品检验检测中心,江苏扬州225000 [2]常熟理工学院生物与食品工程学院,江苏苏州215500

出　　处：《中国药业》2024年第7期79-83,共5页China Pharmaceuticals

基　　金：江苏省市场监督管理局科技计划项目[KJ21125070]。

摘　　要：目的建立测定一次性静脉留置针中双酚A残留量的高效液相色谱-三重四极杆串联质谱法。方法以乙腈为溶剂,超声提取静脉留置针样品中残留的双酚A。色谱柱为Waters Acquity Premier BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为0.05%氨水-甲醇(28∶72,V/V),流速为0.3 mL/min,柱温为30℃,进样量为2μL;三重四极杆质谱,电喷雾电离离子源,负离子、多反应监测模式扫描,气帘气、喷雾气、辅助加热气气压分别为25,55,55 psi,离子化电压为4500 V,定量离子对质荷比(m/z)为227.1/133.0。结果双酚A的质量浓度在5.42~216.8 ng/mL范围内与峰面积线性关系良好(r=0.9999,n=6);检测限为0.1084 ng/mL,定量限为1.084 ng/mL;精密度、重复性试验结果的RSD均小于4.0%;加样回收率为90.44%,RSD为1.27%(n=6)。市售静脉留置针样品中双酚A的残留量最高为9213.34 ng/g。结论该方法操作简便、灵敏度高、重复性好、结果准确,可用于一次性静脉留置针中双酚A残留量的测定。Objective To establish a high-performance liquid chromatography-triple quadrupole tandem mass spectrometry(HPLC-MS/MS)method for the determination of bisphenol A residue in disposable intravenous indwelling needles.Methods Bisphenol A residue was extracted from the intravenous indwelling needle samples by ultrasound with acetonitrile as the solvent.The chromatography column was Waters Acquity Premier BEH C_(18) column(100 mm×2.1 mm,1.7μm),the mobile phase was 0.05% ammonia water-methanol(28∶72,V/V),the flow rate was 0.3 mL/min,the column temperature was 30℃,and the injection volume was 2μL.The triple quadrupole mass spectrometry adopted electric spray ionization ion source with negative ion and multi-reaction monitoring mode for scanning,the pressures of curtain gas,spray gas,auxiliary heating gas were 25,55,and 55 psi,respectively,the ionization voltage was 4500 V,and the mass charge ratio(m/z)of quantitative ion was 227.1/133.0.Results The linear range of bisphenol A was 5.42-216.8 ng/mL(r=0.9999,n=6).The limit of determination(LOD)was 0.1084 ng/mL,and the limit of quantitation(LOQ)was 1.084 ng/mL.The RSDs of precision and repeatability test results were lower than 4.0%.The recovery rate of bisphenol A was 90.44% with an RSD of 1.27%(n=6).The highest content of bisphenol A residue in commercial intravenous indwelling needle samples was 9213.34 ng/g.Conclusion This method is simple,sensitive,reproducible,and accurate,which can be used for the determination of bisphenol A residue in disposable intravenous indwelling needles.

关 键 词：高效液相色谱-三重四极杆串联质谱法 双酚A 一次性静脉留置针 残留量 

分 类 号：R917[医药卫生—药物分析学]