色谱2024，Vol.42Issue(1)：24-37,14.DOI:10.3724/SP.J.1123.2023.04004
超高效液相色谱-三重四极杆质谱法测定水中11大类145种药品和个人护理品
Determination of 145 pharmaceuticals and personal care products in eleven categories in water by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry
摘要
Abstract
Pharmaceuticals and personal care products(PPCPs)are emerging contaminants frequently detected in aquatic environments at trace levels.These chemicals have diverse struc-tures and physicochemical properties and includes pharmaceuticals like antibiotics,antihyper-tensive drugs,antiviral drugs,and psychotropic drugs that are widely used in large quantities worldwide.Considering the large number of pharmaceuticals currently in usage,it is crucial to establish a priority list of PPCPs that should be monitored and/or treated first.An accurate understanding of the occurrence and levels of PPCPs in aquatic environments is essential for providing objective materials for monitoring these emerging contaminants.Therefore,accurate,efficient,sensitive,and high-throughput screening techniques need to be established for deter-mining and quantifying PPCPs. This study developed a method for the determination of 145 PPCPs(grouped into eleven cat-egories:antibiotics,antihypertensive drugs,antidiabetic drugs,antiviral drugs,β-receptor ago-nists,nitroimidazoles,H2 receptor antagonists,psychotropic drugs,hypolipidemic drugs,non-steroidal anti-inflammatory drugs,and others)in water.The method was based on large vol-ume direct injection without sample enrichment and cleanup and used ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS).Water samples were collected and filtered through a 0.22-μm regenerated cellulose(RC)filter membrane.Subsequently,Na2 EDTA was added to the samples to adjust their pH to 6.0-8.0.Internal standards were mixed with the solutions,and because of the addition of Na2 EDTA,the inter-ference of metal ions could be eliminated in the determination of compounds,especially for tet-racycline and quinolone antibiotics.Among the six filter membranes tested in this study(PES,PFTE-Q,PFTE,MCE,GHP,and RC),RC filter membranes were screened for water sample filtration.The UHPLC-MS/MS parameters were optimized by comparing the results of various mobile phases,as well as by establishing the best instrumental conditions.The 145 PPCPs were separated using an Phenomenex Kinetex C18 column(50 mm×3 mm,2.6 μm)via gradient elu-tion.The mobile phases were 0.1%(v/v)formic acid aqueous solution containing 5 mmol/L ammonium formate and acetonitrile for positive ion modes,5 mmol/L aqueous solutions of am-monium formate and acetonitrile for negative ion modes.The samples were quantified using the scheduled multiple reaction monitoring(scheduled-MRM)mode with electrospray ionization in positive and negative ion modes.A standard internal calibration procedure was used to calculate contents of sample.The established method was systematically verified,and it demonstrated a good linear relationship.The average recoveries of the 145 PPCPs at the three spiked levels were in the range of 80.4%-128%with relative standard deviations(RSDs,n=6)of 0.6%-15.6%.The method detection limits(MDLs)ranged from 0.015 to 5.515 ng/L.Finally,the op-timization method was applied to analyze the 145 PPCPs in 11 surface water samples and 6 drinking water samples.Overall,93(64%)out of the 145 analytes were detected.The total con-tents of the PPCPs in surface water samples ranged from 276.9 to 2 705.7 ng/L.The detection frequencies of antidiabetic,antiviral,and psychotropic drugs were 100%.The total contents of the PPCPs in drinking water samples ranged from 140.5 to 211.5 ng/L,and antibiotics,antidia-betic drugs,and antiviral drugs comprised the largest proportion of analytes(by mass concen-tration)in drinking water samples.Our method exhibited high analytical speed and high sensi-tivity.It is thus suitable for the trace analysis and determination of the 145 PPCPs in environ-mental water and showed improved detection efficiency for PPCPs in water,indicating that it has a high potential for practical applications.This study can extend technical support for further pollution-level analysis of PPCPs in water and provide an objective basis for environ-mental management.关键词
超高效液相色谱-三重四极杆质谱/大体积直接进样/药品和个人护理品/环境水体Key words
ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS)/large volume direct injection/pharmaceuticals and personal care products(PPCPs)/environmental water分类
化学化工引用本文复制引用
孙慧婧,张蓓蓓,崔冬妮,董冰洁,王荟,胡冠九..超高效液相色谱-三重四极杆质谱法测定水中11大类145种药品和个人护理品[J].色谱,2024,42(1):24-37,14.基金项目
江苏省环境监测科研基金项目计划(1909,2202) （1909,2202）
2021 年度省级生态环境科研项目(JSZC-G2021-291). Jiangsu Province Environmental Monitoring Research Fund Project(Nos.1909,2202) （JSZC-G2021-291）
Provincial Ecologi-cal and Environmental Research Projects in 2021(No.JSZC-G2021-291). （No.JSZC-G2021-291）
