去磷脂快速萃取-超高效液相色谱-串联质谱法检测人血中双酚A水平

Wei sheng yan jiu = Journal of hygiene research(2018)

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Abstract
目的 建立去磷脂快速萃取-超高效液相色谱-串联质谱法(UPLC-MS/MS)测定人体血液中双酚A水平的检测方法.方法 人体血液样本在酸性条件下通过酶解(β-葡萄糖醛酸酶/硫酸酯酶)和去磷脂固相萃取相结合的方法进行前处理,采用美国五氟苯基液相色谱柱(100mm×3.0mm,2.7μm)分离后,于电喷雾负离子源(ESI-)和多反应监测(MRM)模式下进行测定.结果 双酚A在0.1~ 100 ng/mL质量浓度范围内线性关系良好,R2>0.999,检出限(LOD)为0.05 ng/mL,定量限(LOQ)为0.15 ng/mL.在0.5、5、50 ng/mL加标水平下,平均回收率为87.3%~112.1%.日内和日间精密度分别为3.3% ~ 8.2%,4.9% ~ 10.7% (n =6).结论 该方法灵敏度高、重现性好、回收率高、操作简单,可作为人体血液中双酚A快速检测方法.
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Key words
UPLC-MS/MS,bisphenol A,blood,enzymatic hydrolysis,phospholipid removal
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