SPE-QTOF-MS法快速测定水中4种典型的PPCPs

Rapid Dentification of Pharmaceuticals and Personal Care Products in Water Based on UPLC-QTOF-MS

为了研究水中药品和个人护理品(PPCPs)这一类新兴痕量污染物,利用超高效液相色谱-四极杆-飞行时间质谱(UPLC-QTOF-MS)结合固相萃取技术,建立和优化针对PPCPs的快速筛查和分析方法。将水样经C18固相萃取柱进行前处理,通过考察流动相及柱温箱温度以确定最佳的液相色谱条件;采用一级质谱全扫描模式得到4种PPCPs保留时间、母离子,自发触动二级质谱Target MS/MS得到子离子信息,通过检出限测试和加标回收率实验,确定最佳的质谱条件。结果表明:本方法确定的液相色谱条件和质谱条件下,4种PPCPs的平均回收率在97.33%~106.0%,相对标准偏差小于4.62%。4种PPCP的检出限均小于0.5 ng/mL,定量限均低于2.5 ng/mL,具有较好的灵敏度。

In order to study the emerging contaminants of pharmaceuticals and personal care products(PPCPs)in water,ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS)combined with solid phase extraction(SPE)was used to develop and optimize a rapid screening and analysis method for PPCPs.The water samples were pretreated by C18 solid phase extraction column,and the best liquid chromatography conditions were determined by investigating the mobile phase and the temperature of the column temperature chamber.The retention time and accurate mass of parent ion of four kinds of PPCPs were used for fast screening in full scan mode,while accurate mass of fragment ions was used for confirmation in two-stage Target MS/MS threshold-triggered full mass scan mode.The optimum conditions of mass spectrometry were determined by detection limit test and standard recovery test.The results show that under the conditions of liquid chromatography and mass spectrometry determined by this method,the mean recoveries of the four PPCPs range from 97.33%to 106.0%at different spiked level,and the relative standard deviations are less than 4.62%.The limits of detection(LOD)for the 4PPCPs are all less than 0.5 ng/mL and quantification(LOQ)are all less than 2.5 ng/mL.All of the 4 PPCPs could be well detected in water with excellent sensitivity.