Solid-phase extraction-ultra high-performance liquid chromatography-triple quadrupole mass spectrometry for the determination of 9 nitrosamines in infusion bag extracts
摘要
基于超高效液相色谱串联三重四极杆质谱法(UHPLC-MS/MS)结合固相萃取(SPE)前处理技术,建立了一种测定输液袋提取液中9种亚硝胺的分析方法.样品分别用0.2 mol/L KCl-HCl溶液(pH 3.0)、0.2 mol/L Na2HPO4溶液(pH 10.0)以及20%(V/V)乙醇溶液提取,椰壳活性炭固相萃取柱(CSAC-SPE)前处理,经ZORBAX Eclipse XDB-C18 Rapid Resolution(4.6 mm×150 mm,3.5 µm)色谱柱分离,大气压化学电离离子源正离子(APCI+)结合动态多反应监测模式(dMRM)测定,内标法定量.结果表明,目标物在各自的浓度范围内线性关系良好(r2>0.995),检出限(LOD)为0.50 ng/L,定量限(LOQ)为1.0 ng/L,平均加标回收率为84%～114%,相对标准偏差(RSD)为0.2%～9.2%.对30批输液袋样品的提取液进行检测,6批样品检出N-亚硝基吗啉(NMOR),浓度范围为0.50～1.2 ng/L.本方法实现了输液袋3种提取液(0.2 mol/L KCl-HCl溶液(pH 3.0)、0.2 mol/L Na2HPO4 溶液(pH 10.0)及20%(V/V)乙醇)中9种亚硝胺的同时检测.
An analytical method for the determination of 9 nitrosamines in infusion bag extracts was developed based on ultra high-performance liquid chromatography-tandem triple quadrupole mass spectrometry(UHPLC-MS/MS)combined with solid-phase extraction(SPE)pretreatment.The samples were extracted with 0.2 mol/L KCl-HCl solution(pH 3.0),0.2 mol/L Na2HPO4 solution(pH 10.0),and 20%(V/V)ethanol solutions,respectively,pretreated with coconut shell activated carbon SPE columns(CSAC-SPE),separated on a ZORBAX Eclipse XDB-C18 Rapid Resolution column(4.6 mm×150 mm,3.5 µm),detected under atmospheric pressure chemical ionization in positive ion mode(APCI+)with dynamic multiple reaction monitoring(dMRM),and quantified by internal standard method.The results demonstrated that the target compounds exhibited good linearity within their respective concentration ranges(r2>0.995).The limit of detection(LOD)was 0.50 ng/L,the limit of quantification(LOQ)was 1.0 ng/L,the average spiked recoveries were 84%‒114%,and the relative standard deviations(RSDs)were 0.2%‒9.2%.The extracts of 30 batches of infusion bag samples were analyzed.N-nitrosomorpholine(NMOR)was detected in 6 batches of samples,with the concentration range of 0.50‒1.2 ng/L.The simultaneous detection of 9 nitrosamines in three extracts of the infusion bag(0.2 mol/L KCl-HCl solution(pH 3.0),0.2 mol/L Na2HPO4 solution(pH 10.0),and 20%(V/V)ethanol)were realized by this method.
