液相色谱-串联质谱法测定动物肌肉和牛奶中的雌二醇

Determination of estradiol in animal muscle and milk by liquid chromatography-tandem mass spectrometry

中文关键词:  雌二醇  液相色谱-串联质谱法  丹磺酰氯  衍生

英文关键词:estradiol  liquid chromatography tandem-mass spectrometry  dansyl chloride  derivative

中文摘要:

      目的 建立丹磺酰氯衍生液相色谱-串联四极杆质谱法检测鸡肉、牛肉、牛奶中雌二醇的高灵敏分析方法。方法 酶解后的样品用HLB和氨基固相萃取柱富集净化, 氮气吹干后, 在60 ℃条件下丹磺酰氯衍生 5 min; 以乙腈-水(含0.1%乙酸)为流动相, 采用多离子反应监测正离子模式进行检测。结果 鸡肉、牛肉、牛奶中雌二醇的检出限为0.6 ng/kg, 定量限为2.0 ng/kg, 3个添加水平的平均回收率在82.0%~88.9%之间, 相对标准偏差均小于7.3%。我国6个城市牛肉、鸡肉和牛奶中17-β-雌二醇含量的中位数(平均值)分别为5.51 ng/kg (66.78 ng/kg)、4.60 ng/kg (16.94 ng/kg)和18.00 ng/kg (16.80 ng/kg), 九十百分位数(P90)分别为248.91、39.33和39.60 ng/kg。结论 本方法适用动物肌肉和乳中超痕量雌二醇的含量检测。牛肉、鸡肉和牛奶中17-β-雌二醇的大样本监测数据可为科学的制定残留限量提供必要的数据基础。

英文摘要:

      Objective To establish a highly sensitive analytical method for the determination of estradiol in chicken, beef and milk by dansyl chloride derivative liquid chromatography-tandem quadrupole mass spectrometry. Methods The samples after enzymolysis were enriched and purified by HLB and amino solid-phase extraction columns, dried by nitrogen, and derivatized with dansyl chloride at 60 ℃ for 5 min. Acetonitrile-water (containing 0.1% acetic acid) was used as the mobile phase, and the detection was conducted in a positive ion mode using multi-ion reaction monitoring. Results The detection limit and quantitation limit of estradiol in chicken, beef, and milk were 0.6 ng/kg and 2.0 ng/kg, respectively. The average recoveries of the 3 spiked levels were within the range of 82.0%?88.9%, and the relative standard deviations were all less than 7.3%. The median (mean) values of 17-β-estradiol in beef, chicken, and milk from six cities in China were 5.51 ng/kg (66.78 ng/kg), 4.60 ng/kg (16.94 ng/kg) and 18.00 ng/kg (16.80 ng/kg), respectively, and the ninetieth percentile (P90) values were 248.91, 39.33, and 39.60 ng/kg, respectively. Conclusion This method is suitable for the determination of ultra-trace estradiol in muscle and milk of animals. The large sample monitoring data of 17-β-estradiol in beef, chicken and milk can provide the necessary data basis for the scientific formulation of residue limits.