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目的:建立一种快速、灵敏、准确的牛蛙全血样品中双酚A、4-叔辛基酚和4-壬基酚的超快速液相色谱-串联质谱(UFLC-MS/MS)测定方法。方法:牛蛙全血样品采用蛋白质沉淀法进行净化处理,在Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d.,2.2μm)反相液相色谱柱上进行分离,采用电喷雾离子源(ESI)以高纯氮气(>99.999%)为碰撞气在多反应监测(MRM)模式下进行检测。结果:3种酚类环境雌激素在0.5μg/L～100.0μg/L范围内具有良好的线性(R2>0.999),检出限在0.07μg/L～0.15μg/L范围,最低定量限在0.20μg/L～0.46μg/L范围,RSDs在3.9%～8.2%范围;在加标水平为1.0μg/L、10.0μg/L和50.0μg/L时,3种酚类环境雌激素在牛蛙全血中的回收率分别在97%～106%、93%～109%、94%～96%范围。结论:本方法可用于牛蛙全血样品中酚类环境雌激素的测定。
OBJECTIVE: To establish a rapid, sensitive and accurate method for the determination of bisphenol A, 4-tert-octylphenol and 4-nonylphenol in whole blood samples of bullfrog by UFLC-MS / MS . Methods: Whole blood samples of bullfrog were purified by protein precipitation and separated on a Shim-pack XR-ODS II (100 mm × 2.0 mm id, 2.2 μm) reverse phase liquid chromatographic column. Electrospray ionization (ESI) High-purity nitrogen gas (> 99.999%) was used as collision gas in multiple reaction monitoring (MRM) mode. Results: The three estrogenic phenols showed a good linearity (R2> 0.999) in the range of 0.5μg / L to 100.0μg / L with the detection limit of 0.07μg / L ~ 0.15μg / L, the lowest limit of quantitation The RSDs ranged from 0.20μg / L to 0.46μg / L, and the RSDs ranged from 3.9% to 8.2%. When the spiked levels were 1.0μg / L, 10.0μg / L and 50.0μg / L, The recovery rates in whole blood ranged from 97% to 106%, 93% to 109% and 94% to 96%, respectively. Conclusion: This method can be applied to the determination of phenolic environmental estrogen in bullfrog whole blood samples.