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目的建立测定人血浆中10种环境酚类物质的同位素内标-液液萃取-超高压液相色谱串联质谱测定法。方法样品经酶消解后,采用不同萃取剂进行液液萃取前处理,以含甲酸的甲醇和水为流动相,以梯度洗脱方式用C18色谱柱对目标化合物进行分离。以负离子喷雾模式电离,多反应离子监测方式进行定性及定量检测。结果该方法检测双酚A、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、对羟基苯甲酸庚酯和对羟基苯甲酸苯酯、对羟基苯甲酸、3,4-二羟基苯甲酸和三氯生在0.05~50 ng/ml范围内满足线性需要(r=0.999)。经同位素内标校正后,酶消解-乙酸乙酯液液萃取法对10种目标化合物在两个浓度水平下的加标回收率均在90%~110%,最低检出限为0.03~0.15 ng/ml,定量限为0.10~0.50 ng/ml,日内和日间RSDs<10%。结论该方法对人血浆中10种环境酚类化合物的测定具有较高的灵敏度和精确性,可满足上述化学品的人体暴露监测需要。
Objective To establish an isotope internal standard for the determination of 10 environmental phenols in human plasma by liquid-liquid extraction and ultra-high pressure liquid chromatography-tandem mass spectrometry. Methods Samples were digested by enzymes and pretreated by liquid-liquid extraction with different extractants. The mobile phase consisted of methanol and water containing formic acid. The target compounds were separated by gradient elution on a C18 column. Ionization spray mode ionization, multi-reactive ion monitoring methods for qualitative and quantitative detection. Results The method for the determination of bisphenol A, methyl paraben, ethyl paraben, propyl paraben, butyl paraben, p-hydroxybenzoate and p-hydroxybenzoate, Parabens, 3,4-dihydroxybenzoic acid and triclosan satisfied the linearity requirement (r = 0.999) within the range of 0.05-50 ng / ml. After calibration by isotope internal standard, the spiked recoveries of 10 target compounds were 90% -110% at the two concentration levels by enzymatic digestion-ethyl acetate liquid-liquid extraction with the detection limit of 0.03-0.15 ng / ml, with a limit of quantification of 0.10 to 0.50 ng / ml with intraday and daytime RSDs <10%. Conclusion This method has high sensitivity and accuracy for the determination of ten environmental phenolic compounds in human plasma and can meet the needs of human exposure monitoring of the above chemicals.