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

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...

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

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.