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目的建立液相-串联质谱法(LC-MS/MS)测定牛奶中雌二醇残留的分析方法。方法样品经甲醇提取,离心,过CARB/NH2复合柱净化,氮吹至干,用1 ml乙腈-水(4∶6,V∶V)定容后经超高效液相色谱分离,电喷雾串联四级杆质谱进行检测,内标法定量。结果本法雌二醇在3.0μg/L~60μg/L的范围内线性关系良好,r=0.9992,平均回收率为91.2%~109.5%,相对标准偏差为3.45%~6.21%。方法定量限1.0μg/kg。结论该方法快速、灵敏,适用于批量实际样品检测。
Objective To establish a method for the determination of estradiol residues in milk by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods The samples were extracted by methanol, centrifuged, cleaned up by CARB / NH2 composite column, the mixture was purged with nitrogen and fixed with 1 ml of acetonitrile-water (4: 6, V: V) Four rod mass spectrometry for detection, internal standard method. Results The estradiol showed a good linearity in the range of 3.0μg / L ~ 60μg / L with the average recovery of 91.2% ~ 109.5% and the relative standard deviation of 3.45% ~ 6.21%. Methods Quantitative limit 1.0μg / kg. Conclusion The method is fast and sensitive and suitable for batch real sample testing.