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超高效液相色谱-串联质谱法同时快速测定食用油中9种外源性杂质成分
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罗辉泰,黄晓兰,吴惠勤,张秋炎,朱志鑫,黄芳,林晓珊,马叶芬,邓欣 广东省测试分析研究所广东省化学危害应急检测技术重点实验室广东省中药质量安全工程技术研究中心 
基金项目:国家重点研发计划资助项目(2017YFB0306501)
中文摘要:建立了超高效液相色谱-串联质谱同时快速测定食用油中9种外源性杂质成分的分析方法。样品经乙腈涡旋提取后,采用XSelectHSS PFP(100 mm×2.1 mm,3.5 μm)色谱柱,以5 mmol/L甲酸铵-乙腈为流动相进行梯度洗脱,在10 min内实现9种待测物的良好分离。在电喷雾正离子模式下,以多反应监测(MRM)模式采集数据并作定性鉴别和定量分析。结果表明,9种待测物在相应的质量浓度范围内线性关系良好,相关系数(r2)均大于0.996;在3个不同浓度加标水平下,平均回收率为68.2%~104%,相对标准偏差(RSD)为2.2%~12%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.02~0.10 μg/kg及0.05~0.25 μg/kg。结果表明,该法简单、快速、灵敏、准确、可靠,适用于食用油中9种难挥发外源性特征杂质的同时快速定性和定量分析。
中文关键词:超高效液相色谱-串联质谱(UHPLC-MS/MS)  食用油  外源性杂质  辣椒素  胡椒碱  6-姜酚  羟基-α-山椒素
 
Simultaneous and Rapid Determination of Nine Exogenous Impurities in Edible Oils by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A comprehensive analytical method was developed and validated for the simultaneous and rapid determination of nine exogenous impurities in edible oils by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The analytes in sample were extracted with acetonitrile using vortex mixer.The chromatographic separation was performed on an XSelect-HSS PFP chromatographic column(100 mm×2.1 mm,3.5 μm),with 5 mmol/L ammonium formate and acetonitrile as mobile phases by gradient elution.The qualitative and quantitative analyses were performed by electrospray ionization mass spectrometry in positive mode under multiple reaction monitoring(MRM) mode.Results showed that there were good linear relationships for nine analytes in corresponding concentration range with their correlation coefficients(r2) larger than 0.996.Average recoveries for 9 analytes in sample at three spiked levels ranged from 68.2% to 104%,with relative standard deviations(RSD) of 2.2%-12%.The limits of detection(LOD,S/N≥3) and quantitation(LOQ,S/N≥10) were in the ranges of 0.02-0.10 μg/kg and 0.05-0.25 μg/kg,respectively.The established method is simple,rapid,sensitive,accurate and reliable,and is suitable for the simultaneous and rapid determination of nine exogenous characteristic impurities in edible oils.
Key Words:ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)  edible oils  exogenous impurities  capsaicin  piperine  6-gingerol  hydroxy-α-sanshool
引用本文:罗辉泰,黄晓兰,吴惠勤,张秋炎,朱志鑫,黄芳,林晓珊,马叶芬,邓欣.超高效液相色谱-串联质谱法同时快速测定食用油中9种外源性杂质成分[J].分析测试学报,2019,(5):532-538.
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