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    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

    • 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ACQUITYTM BEH C18色谱柱分离,用含0.1%(体积分数)甲酸的5 mmol·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0.2~0.3 μg·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 %。

       

      Abstract: 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 C18 chromatographic column was used for separation, using the mixed solutions of 5 mmol·L-1 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 RSD′s (n=6) were found in the ranges of 76.2%-108.3% and 4.3%-11.7%, respectively.

       

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