固相萃取-液相色谱-串联质谱法测定水中的6种雌激素

Determination of 6 estrogens in water by liquid chromatography-tandem mass spectrometry

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 develop a method of the determination of 6 estrogens in water by solid phase extraction（ SPE） and liquid chromatography tandem mass spectrometry（ LC- MS / MS）. Methods 6 estrogens were determined in water by the pretreatment technology of solid phase extraction and LC- MS / MS. Liquid chromatography selected C18 column as the separation column. Methanol,acetonitrile and water were adopted as mobile phase for gradient elution,and tandem mass spectrometry was adopted for detection in multi- reaction monitoring mode. MS,HPLC and SPE condition were optimized in this experiment. The method was applied to detect 10 cases of tap waters. Results Good linearity was obtained when the concentration of 6 estrogens was among 0 ng / L- 5 000 ng / L（ r 〉0. 995）. The detection limit of quantification was among 8. 68 ng / L- 103 ng / L,and the recoveries were among 80. 3%- 93. 0%. And the relative standard derivations（ RSDs） were ≤ 15. 5%. Conclusion The method has the advantages of sensitivity,selectivity and accuracy. And it can be used to simultaneously determine 6 estrogens in water.