分散固相萃取-超高效液相色谱串联质谱法测定 土壤中雌酮、雌二醇和乙炔基雌二醇

Determination of estrone, 17β-estradiol and 17α-ethinylestradiol in soil by ultra-high performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction

中文关键词:  土壤  分散固相萃取  超高效液相色谱串联质谱法  雌酮  雌二醇  乙炔基雌二醇

英文关键词:soil  dispersive solid phase extraction  ultra-high performance liquid chromatography-tandem mass spectrometry  estrone  17β-estradiol  17α-ethinylestradiol

中文摘要:

      目的 建立土壤中雌酮、雌二醇和乙炔基雌二醇的超高效液相色谱串联质谱法(UPLC-MS/MS)测定方法。方法 土壤样品经乙腈提取和PSA+C18分散固相萃取, 采用UPLC-MS/MS多反应模式(MRM)进行分析测定, 流动相为甲醇/乙腈(50:50, V:V)和0.1%氨水。结果 雌酮、雌二醇和乙炔基雌二醇在1~200 μg/kg范围内呈现良好线性, 相关系数(r2)均不低于0.9974, 方法的检出限(S/N=3)分别为0.0012、0.0036和0.0058 μg/kg。土壤中10、50和500 μg/kg 3个添加水平下的回收率为82.9~103.6%, RSD小于7.7。结论 该方法简便、快速、灵敏且节省溶剂, 适于土壤中雌激素物质的检测。

英文摘要:

      Objective To establish a method for the determination of estrone, 17β-estradiol and 17α-ethinylestradiol in soil by ultra-high performance liquid chromatography-tandemmass spectrometry (UPLC-MS/MS). Method According to dispersive solid phase extraction method, the soil samples were extracted by acetonitrile, purified by PSA+C18 and analyzed by UPLC-MS/MS under the multiple reaction monitoring (MRM) mode with methanol/acetonitrile(50:50, V:V) and 0.1% ammonia water as mobile phase. Results Good linear relationships were obtained in the concentration range of 1.0~200 μg/kg with high correlation coefficients over 0.9974, and the limits of detection and quantification for 3 kinds of estrogens were 0.0012, 0.0036 and 0.0058 μg/kg, respectively. The average recoveries ranged from 82.9% to 103.6% under the addition levels of 10, 50 and 500 μg/kg and the relative standard deviation was below 7.7%. Conclusion This method is simple, rapid, sensitive and solvent saving, which is suitable for the determination of estrogens in soil samples.