四极杆/静电场轨道阱高分辨质谱法测定桶装水中的9种塑化剂  

Detection of 9 phthalate acid esters in water by quadrupole/electrostatic field high resolution mass spectrometry

作　　者：唐晓琴[1] 甘源[1] 覃梅[1] 贺丽迎 李莉 周春艳[1] TANG Xiao-qin;GAN Yuan;QIN Mei;HE Li-ying;LI Li;ZHOU Chun-yan(Chongqing Center for Disease Control and Prevention,Chongqing 400042,China)

机构地区：[1]重庆市疾病预防控制中心

出　　处：《中国卫生检验杂志》2019年第20期2478-2480,2523,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立桶装水中9种塑化剂的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q Extractive)联用的测定方法。方法由于该方法的灵敏度较高,样品可以不经过任何前处理操作,直接上机分析测试。液相部分采用BEHC18色谱柱(50mm×2.0mm,2.1μm)分离,以甲醇-0.1%甲酸水溶液作为流动相,梯度洗脱。质谱分析则采用电喷雾电离源正离子模式(HESI+)在t-SIM扫描模式下检测,通过理论精确质量数与所测得的精确质量数之间的匹配度和保留时间作为定性判断标准,以外标法定量。结果9种塑化剂在1.0μg/L^16.0μg/L时均呈现良好的线性关系,相关系数为0.998~0.999,9种塑化剂的检出限为0.1μg/L,加标回收率为62.3%~112.8%,相对标准偏差为1.1%~8.5%。结论该方法具有操作简便,灵敏度高,重现性好等特点,可满足桶装水样品中PAEs检测的要求。Objective To develop a method for the detection of 9 phthalate acid esters in water by ultra-high-performance liquid chromatography-quadrupole/electrostatic field high resolution mass spectrometry(UPLC-Q Extractive).Methods The water samples were detected by QE directly without any sample processing for the high sensitivity.The separation was performed on a BEH C18 column(50 mm×2.0 mm,2.1μm)by a mobile phase consisting of methanol-acetonitrile-0.1%formic acid aqueous solution under gradient elution.The detection was carried out in positive electrospray ionization and targeted-selected ion monitor mode.The targeted compounds were confirmed by the difference between theoretical accurate molecular mass and the actual accurate molecular and the retention time.The quantitative analysis was carried out with external standard method.Results Good linearity was obtained when the concentration of the standard solution of phthalate acid esters was within 1.0μg/L-16.0μg/L.The correlation coefficients were within 0.998-0.999.The detection limits for phthalate acid esters was 0.2μg/kg,and the average recoveries were within 62.3%-112.8%.The relative standard deviations(RSDs)were within 1.1%-8.5%.Conclusion This method is simple,fast,accurate and reproducible for the determination of 9 phthalate acid esters in water samples.

关 键 词：四极杆/静电场轨道阱高分辨质谱法 塑化剂 桶装水 

分 类 号：R123.1[医药卫生—环境卫生学]