气相色谱-质谱法同时检测婴幼儿配方奶粉中的6种雌激素残留  

Effective Separation and Simultaneous Determination of Six Estrogen Residues in Infant Formula by GC-MS

作　　者：孙汉文[1] 李挥[1,2] 康占省[1] 张敬轩[1,2] 吕运开[1] 

机构地区：[1]河北大学化学与环境科学学院,河北省分析科学重点实验室,河北保定071002 [2]河北省食品质量监督检验研究院,河北石家庄050051

出　　处：《河北大学学报（自然科学版）》2011年第6期607-611,共5页Journal of Hebei University(Natural Science Edition)

基　　金：河北省自然科学基金资助项目(B2008000583);河北省科技支撑项目(09227134D,10967126D)

摘　　要：建立了婴幼儿配方奶粉中6种雌激素残留(己烯雌酚diethylstilbesterol,17α-乙炔基雌二醇17α-ethynylestradiol,17α-雌二醇17α-estradiol,17β-雌二醇17β-estradiol,雌三醇estriol,雌酮estrone)的气相色谱-质谱(GC-MS)的检测方法.样品经酶解后,用乙腈超声提取.提取液蒸发至近干,五氟丙酸酐(PFPA)衍生化后,经HP-5MS弱极性色谱柱分离,在SIM模式下进行定性分析和定量检测.结果表明:在0.1～50ng/mL内,6种药物的校准曲线呈现良好的线性,相关系数(r)大于0.999.17α-乙炔基雌二醇的定量限为0.8μg/kg,其余5种的定量限为0.1μg/kg.6种药物在3.0,5.0,10.0μg/kg质量浓度添加水平下,其平均回收率为60.6%～120.6%;相对标准偏差(RSD)为7.8%～19.6%.该方法已成功应用于婴幼儿配方奶粉中6种雌激素残留的定性定量检测.New method had been developed for effective separation and simultaneous determination of six estrogen residues including diethylstilbesterol,17α-ethynylestradiol,17α-estradiol hemihydrate,17β-estradiol hemihydrate,estriol and estrone in infant formula by gas chromatography-mass spectrometry（GC-MS）.The infant formula samples were enzymatically digested with β-glucuronidase/arylsulfatase,and then extracted with acetonitrile by ultrasonication.This process was repeated two times and the extracts were combined.The combined extracts were evaporated to dryness.The estrogens in the residue were derivated with pentafluoropropionic anhydride.Six estrogen residues were measured with GC-MS using electron impact ionization source in SIM mode.Gas chromatographic separation was performed on a HP-5MS capillary column（30 m × 0.25 mm internal diameter;0.25 μm film thickness）.The baseline separation of two isomers（17α-estradiol hemihydrate and 17β-estradiol hemihydrate） of estradiol was achieved by optimizing the heating process.The calibration curves showed good linearity with correlation coefficient（r） of 0.999.The limits of quantification（LOQ） of six estrogens ranged from 0.1 to 0.8 μg/kg.Experiments on spiked infant formula samples showed that at spiked level of 3.0,5.0 and 10.0 μg/kg,the mean recoveries were within 60.6%-120.6%,and the relative standard deviations ranged from 7.8% to 19.6%.This method had been successfully used for the qualitatively and quantitatively determination of the six estrogen residues in infant formula.

关 键 词：气相色谱-质谱 雌激素 奶粉 

分 类 号：O657.7[理学—分析化学]