超高效液相色谱-串联质谱法测定肉制品中8种雌激素残留量  

UHPLC-MS/MS Determination of Residual Amounts of 8 Estrogens in Meat Products

作　　者：耿金培 曹鹏[1,2] 梁君妮 徐英江[3] 李晓玉 李金强 沙美兰 牟妍 

机构地区：[1]烟台出入境检验检疫局,烟台264000 [2]山东农业大学食品科学与工程学院,泰安271018 [3]山东省海洋水产研究所,烟台264006

出　　处：《理化检验（化学分册）》2012年第12期1398-1402,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：山东检验检疫局科技计划项目(SK200919)

摘　　要：提出了超高效液相色谱-串联质谱法测定肉制品中8种雌激素(辛基酚、壬基酚、双酚A、己烯雌酚、雌酮、17β-雌二醇、17α-乙炔雌二醇和雌三醇)含量的方法。样品经乙酸乙酯提取两次,过HLB固相萃取柱净化后,将洗脱液氮吹至近干,残渣用甲醇-水(1+9)溶液溶解。采用AC-QUITYTMBEH C18色谱柱分离,用含0.1%(体积分数)甲酸的5mmol.L-1乙酸铵溶液和甲醇组成的流动相梯度洗脱。质谱测定中采用负离子电离方式,多反应监测模式。方法检出限(3S/N)在0.2～0.3μg.kg-1之间。方法的回收率在76.2%～108.3%之间,测定值的相对标准偏差(n=6)为4.3%～11.7%。UHPLC MS/MS was applied to the determination of residual amounts of 8 kinds of estrogens, including octylphenol, 4 nonylphenol, bishphenol A, diethylstilbestrol, estrone, 17β-estradiol, 17α ethinylestradiol and estriol, in meat products. The sample was extracted twice with acetic ether, which was concentrated and purified by HLB solid-phase extraction column. The eluate was evaporated to near dryness by N2-blowing and the residue was dissolved with methanol-water （1 ＋ 9 ）. ACQUITYTM BEH C18chromatographic column was used for separation, using the mixed solutions of 5 mmol · L ^- ammonium acetate （containing φ 0. 1% formic acid） and methanol as mobile phase in the gradient elution. ESI with negative ionization mode and multi-reactions monitoring mode were used in the MS/MS analysis. Values of detection limits （3S/N） found were in the range of 0. 2--0. 3 μg·kg^-1. Values of recovery and RSI）＇s （n--6） were found in the ranges of 76. 2%-108. 3% and 4. 3%--11.7%, respectively.

关 键 词：超高效液相色谱-串联质谱法 肉制品 雌激素 

分 类 号：O657.63[理学—分析化学]