液相色谱-串联质谱法快速测定环境水中四溴双酚A

Determination of tetrabromobisphenol A in enviromental water by liquid chromatography coupled with tandem mass spectrometry

目的建立环境水中四溴双酚A的固相萃取-超快速液相色谱-串联质谱(SPE-UFLC-MS/MS)分析方法。方法水样经HLB小柱净化、浓缩后分析。以乙腈-水(含0.04%氨水)为流动相,采用梯度洗脱在Shim-pack XR-ODSⅡ色谱柱(2.0 mm×150 mm, 2.2μm)上进行分离,流速为0.45 ml/mim,串联质谱在电喷雾(ESI)离子多反应监测(MRM)模式下检测,以保留时间以及特征离子对定性,内标法定量。结果四溴双酚A在1.00μg/L～100.0μg/L浓度内呈良好线性关系。方法检出限为0.03μg/L,定量限为0.1μg/L。平均回收率为96.2%～105.0%,相对标准偏差(RSD)为1.8%～3.1%。结论本法分析速度快、重现性好、灵敏度高,可用于环境水中四溴双酚A的分析测定。

Objective To establish an ultrafast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) for the determination of tetrabromobisphenol A in environmental water. Methods The water sample was purified and concentrated with HLB cartridge. The UFLC separation was performed on a Shim-pack XR-ODSⅡ column(2.0 mm×150 mm, 2.2 μm) with a linear gradient elution program of acetonitrile and water(0.04% NH4OH) as the mobile phase, and the flow rate was 0.45 ml/min. The analyte was separated and detected by liquid chromatography and electrospray ionization-mass spectrometry in multiple reaction monitoring(MRM) mode. The qualitative analysis was based on the retention time and characteristic ion pairs of the analyte. The quantitative analysis was based on internal standard curve. Results Good linearity was obtained when the concentration of tetrabromobisphenol A was within 1.00 μg/L-100.0 μg/L. The limit of quantification(LOQ) was 0.1 μg/L and the recoveries were within 96.2%-105.0%, with the relative standard deviations(RSDs) of 1.8%-3.1%. Conclusion The method is quick, reproducible, sensitive and suitable to the determination of tetrabromobisphenol A in environmental water.