UPLC-MS/MS法同时测定人尿中12种多环芳烃代谢物

张婧婧; 朱峰; 刘华良

doi:10.13421/j.cnki.hjwsxzz.2020.06.014

UPLC-MS/MS法同时测定人尿中12种多环芳烃代谢物

Simultaneous Determination of 12 Polycyclic Aromatic Hydrocarbon Metabolites in Human Urine by UPIC-Ms/Ms

摘要

摘要:
目的建立可以同时测定人尿中12种多环芳烃代谢物的超高效液相色谱串联质谱（UPLC-MS/MS）法。
方法人尿样品经β-葡萄糖苷酸酶水解，C₁₈固相萃取柱净化，氮吹浓缩，甲醇-水（40：60，v/v）溶解后，以甲醇-水为流动相，梯度洗脱，采用WATERS ACQUITY^® BEH C₁₈（2.1 mm×100 mm，1.7 μm）色谱柱分离，电喷雾离子化负离子检测12种多环芳烃代谢物的含量。
结果人尿多环芳烃代谢物浓度在（0.002 5~5）ng/mL范围内线性相关系数均>0.99，方法检出限为（0.001~0.1）ng/mL，低（0.04 ng/mL）、中（0.40 ng/mL）、高（2.00 ng/mL）3种浓度的加标回收率均>90%，精密度良好（RSD < 10%）。
结论该方法灵敏度和回收率高、精密度好，可同时测定人尿中12种多环芳烃代谢物。

Abstract:
Objective To develope an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous determination of 12 polycyclic aromatic hydrocarbon (PAH) metabolites in human urine.
Methods The human urine samples were hydrolyzed by β-glucuronidase, purified by a C₁₈ solid-phase extraction column, concentrated by nitrogen, and dissolved by methanol-water (40:60, v/v), and then the samples were separated by a WATERS ACQUITY^® BEH C₁₈ column (2.1 mm×100 mm, 1.7 μm) with a mobile phase of methanol-water for gradient elution, and electrospray ionization was used to measure the content of 12 PAH metabolites.
Results The PAH metabolites in human urine samples showed a good linear relationship within the concentration range of (0.002 5~5) ng/mL, with a correlation coefficient of > 0.99, and the detection limit was (0.001~0.1) ng/mL. The average recoveries of PAH metabolites in low (0.04 ng/mL), medium (0.40 ng/mL), and high (2.00 ng/mL) were above 90%, with good precision (relative standard deviation < 10%).
Conclusion This method has high sensitivity, high recovery, and good precision and can be used for the simultaneous determination of 12 PAH metabolites in human urine.

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