高效液相色谱-串联质谱法同时测定植物油中苯并芘与黄曲霉毒素B_1,B_2,G_1,G_2  

Simultaneous Determination of Benzo(a)pyrene and Aflatoxins(B_1,B_2,G_1,G_2) in Vegetable Oil by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王浩[1] 杨红梅[1] 郭启雷[1] 赵丽[1] 史海良[1] 潘红艳[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《分析测试学报》2014年第8期911-916,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科研项目(2012QK011)

摘　　要：建立了植物油中苯并芘和黄曲霉毒素B1,B2,G1,G2的高效液相色谱-串联质谱测定方法.以乙酸乙酯-环己烷（1∶1）提取样品,凝胶渗透色谱净化,以XDB-C18色谱柱（4.6 mm×50 mm,1.8 μm）分离,流动相为甲醇（含1％甲苯）和10 mmol/L乙酸铵水溶液（梯度洗脱）,流速0.25 mL/min,大气压光致电离（APPI＋）,多反应监测模式扫描（MRM）,外标法定量.结果表明,苯并芘和黄曲霉毒素B1,B2,G1,G25种化合物分别在0.3～25,0.5 ～30,1.0～10,1.0～30,1.0～10 μg/kg范围内呈良好线性,相应定量下限分别为0.3,0.5,1.0,1.0,1.0 μg/kg,相关系数为0.9996～0.9999;加标回收率为80.3％～106.8％,相对标准偏差为4.0％～10.0％.该方法操作简单、测定结果准确,可用于植物油中苯并芘和黄曲霉毒素B1,B2,G1,G2的同时快速测定.A liquid chromatography-tandem mass spectrometric （LC-MS/MS） method was developed for the simultaneous determination of benzo（a） pyrene and aflatoxins（B1,B2,G1,G2） in vegetable oil.The sample was extracted with ethyl acetate-hexane （1 ∶ 1）,cleared up by GPC.The separation of target compounds were performed on an XDB C18 column（4.6 mm ×50 mm,1.8 μm）at 25 ℃ with methanol and 10 mmol/L ammonium acetate solution as mobile phase by gradient elution at a flow rate of 0.25 mL/min.Then the samples were ionized using atmospheric-pressure photoionization ion source ionization,examined under multiple reaction monitoring（MRM） mode and quantiffed by the external standard method.The quantitation limits of benzo（a） pyrene and aflatoxins（B1,B2,G1,G2） were 0.3,0.5,1.0,1.0,1.0 μg/kg,respectively.The linear ranges of benzo （a）pyrene and aflatoxins（B1,B2,G1,G2） were 0.3-25,0.5-30,1.0-10,1.0-30,1.0-10 μg/kg,respectively,with correlation coefficients（r） of 0.999 6-0.999 9.The spiked recoverie of target compounds in vegetable oil were in the range of 80.3％-106.8％,with relative standard deviations of 4.0％-10.0％.The real sample tests showed that the method was simple and accurate,and could be used for the determination of benzo（a）pyrene and aflatoxins（B1,B2,G1,G2） in vegetable oil.

关 键 词：液相色谱串联色谱 凝胶渗透色谱 苯并芘 黄曲霉毒素 植物油 

分 类 号：O657.63[理学—分析化学] S852.44[理学—化学]