超高效液相色谱-四级杆串联质谱法检测饮用水中双酚A和双酚F及其氯化消毒副产物

Simultaneous determination of bisphenol A,bisphenol F and their chlorinated byproducts in drinking water by ultra-performance liquid chromatography-tandem mass spectrometry

目的建立饮用水中双酚A(BPA)、双酚F(BPF)及其9种氯化消毒副产物的超高效液相色谱-四级杆串联质谱(UPLC-MS/MS)检测方法。方法 500 ml饮用水样品经PLEXA固相萃取柱富集净化后,通过BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm)分离,以乙腈-水作为流动相梯度洗脱,采用四极杆串联质谱仪电喷雾负离子模式进行检测,外标法定量。结果 11种目标物质在给定的浓度范围内具有良好的线性关系(r^2>0.99),方法定量限(LOQ)为0.01~4.00 ng/L,加标回收率为78.8%~99.6%,相对标准偏差(RSD)均小于12.2%。利用该方法分析40份实际饮用水样品,BPA、BPF和四氯双酚A(4Cl-BPA)3种目标物质在样品中的检出率分别为45.0%(18/40)、40.0%(16/40)和32.5%(13/40),检出浓度分别为0.60~9.40、<LOQ^106.20和<LOQ^0.02 ng/L。结论本方法具有良好的灵敏度、回收率和重复性,适合饮用水样品中BPA、BPF及其氯化消毒副产物的测定。

Objective A analytical method was developed to determine bisphenol A（BPA）,bisphenol F（BPF）and their chlorinated products in drinking water using ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.Methods Water samples were concentrated and purified with PLEXA solid-phase extraction catridges.The target analytes were separated on a BEH C（18）column（2.1 mm × 100 mm,1.7 μm） with gradient elution using acetonitrile and water,and identified under negative electrospray ionization.The matrix-matched standard calibration curves were used for the quantitative analysis.Results Good linearities were achieved for all analytes with correlation coefficient（r-2） above 0.99.The quantitation limits of the method（LOQ） were in the ranges of0.01-4.00 ng/L.The recoveries of the target analytes ranged from 78.8%-99.6%,with relative standard deviations（RSD） less than 12.2%.Forty drinking water samples were analyzed by the developed method,and the detection rate of BPA,BPF and 4Cl-BPA were 45.0%（18/40）,40.0%（16/40） and 32.5%（13/40）,the concentrations were0.60-9.40 ng/L, LOQ-106.20 ng/L and LOQ-0.02 ng/L.Conclusion The established method could be applied in the simultaneous determination of BPA,BPF and their chlorinated products in drinking water due to its excellent sensitivity,recovery and reproducibility.