超高效液相色谱—三重四级杆质谱串联法测定餐厨废油中黄曲霉毒素B_1、B_2、G_1、G_2的研究  

Determination of aflatoxins in waste cooking oil by liquid chromatography- tandem mass spectrometry

作　　者：廖权丰[1,2] 周芳梅[1,2] 叶日金[3,2] 

机构地区：[1]广东省食品质量监督检验站,广州510308 [2]广东省食品工业公共实验室,广州510308 [3]广东省食品工业研究所,广州510308

出　　处：《中国食品添加剂》2013年第5期193-197,共5页China Food Additives

基　　金：广东省科技计划项目(2010A040301013)

摘　　要：建立了餐厨废油中黄曲霉毒素B1、B2、G1、G2的超高效液相色谱-三重四级杆质谱串联法(UPLC-MS-MS)测定方法。试样中的黄曲霉毒素经70%甲醇-水溶液超声提取、黄曲霉毒素免疫亲和柱萃取柱净化并浓缩,用流动相溶解进行UPLC-MS-MS测定。结果表明,液质联用法对餐厨废油中黄曲霉毒素的检测限为0.5μg/kg,标准工作液在0.5 25μg/L的范围内线性良好,相关性系数在0.9990 0.9994。加标浓度在1.0 20μg/L范围内,餐厨废油中黄曲霉毒素的回收率在78.6%103%之间,相对标准偏差≤9.1%,能够满足快速无残留检测要求,可较好地用于餐厨废油中黄曲霉毒素B1、B2、G1、G2的检测及假阳性的判别。To tally Total of 4 aflatoxins in waste cooking oil were determined by ultra performance liquid chromatography combined with electro spray ionization triple quadrupole tandem mass spectrometry （UPLC-MS/MS） under the multiple reaction monitoring （MRM） mode,and especially focused on the optimization o f extraction,clean-up,HPLC separation and MS/MS parametersof analytes.The aflatoxins B1,B2,G1 and G2were extracted by 70％ of methanol aqueous solution,purified by passing through multifunctional cartridges.The elution was evaporated by nitrogen blow and dissolved by mobile phase and,and then assayed deteced by UPLC-MS/ MS.The limits of detection （LOD）are were 0.5μg · kg-1.The calibration curves are were linear between 0.5μg · L-1 and 25μg · L-1 for aflatoxins B1,B2,G1 and G2,the correlation coefficients were in the ranger of 0.9990 ～ 0.9994.Recoveries of the aflatoxins in waste cooking oil are were 78.6％ ～103％,and inter-relative standard deviation （n =6） is was less than 9.1％ at spiked level of 1.0 ～20μg · kg-1.

关 键 词：液相色谱 质谱 黄曲霉毒素 餐厨废油 

分 类 号：TS207.3[轻工技术与工程—食品科学]