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目的建立水中6种雌激素的固相萃取-液相色谱-串联质谱检测方法。方法利用固相萃取前处理技术,液相色谱串联质谱的方法测定水中6种雌激素。液相色谱选择C_(18)色谱柱作为分离柱,甲醇、乙腈和水作为流动相梯度洗脱,串联质谱多反应监测模式进行检测。实验方法优化了质谱条件、液相色谱条件和固相萃取前处理条件。应用该方法测定了10份自来水样品。结果 6种雌激素在0 ng/L~5 000 ng/L时呈良好的线性关系,相关系数>0.995,定性检出限为8.68 ng/L~103 ng/L,回收率为80.3%~93.0%,相对标准偏差(RSD)均≤15.5%。结论本方法不但可以同时测定水中6种雌激素,而且具有灵敏度好、选择性好、准确度高等优点。
Objective To establish a method for the determination of six estrogens in water by liquid chromatography-tandem mass spectrometry. Methods Six kinds of estrogen in water were determined by solid phase extraction pretreatment and liquid chromatography tandem mass spectrometry. Liquid chromatography column C_ (18) was used as the separation column, and methanol, acetonitrile and water were used as the mobile phase gradient elution, and tandem mass spectrometry was used for the detection of multiple reaction monitoring. The experimental method optimizes the conditions of mass spectrometry, liquid chromatography and pre-solid phase extraction. Ten tap water samples were measured using this method. Results The results showed that there was a good linear relationship between 6 estrogen and 0 ng / L ~ 5000 ng / L, the correlation coefficient was> 0.995, the detection limit was 8.68 ng / L ~ 103 ng / L and the recovery was 80.3% ~ 93.0 %, Relative standard deviation (RSD) ≤15.5%. Conclusion This method not only can simultaneously determine six kinds of estrogen in water, but also has the advantages of good sensitivity, good selectivity and high accuracy.