摘要
提出了固相萃取-液相色谱-串联质谱法(LC-MS/MS)测定生活污水中甲氧苄啶、马来酸氯苯那敏、异丙安替比林、安替比林、非那西丁、苯海拉明、甲芬那酸、地西泮、酮洛芬等9种痕量常用非甾体类药物的方法。将污水样品用0.45μm玻璃纤维滤膜过滤,收集1.0 L水样,加入2.5 g乙二胺四乙酸二钠(Na2EDTA),振摇5 min,以10 mL·min^(-1)的速率过HLB固相萃取柱(预先分别用5 mL甲醇、5 mL水进行活化),用5 mL水淋洗,用5 mL甲醇洗脱,收集洗脱液用氮气吹至近干,残渣用20%(体积分数)甲醇溶液1.0 mL复溶,涡旋混匀1 min,过0.2μm滤膜。液相色谱分离采用BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以不同体积比的含0.1%(体积分数,下同)甲酸的乙腈溶液-0.1%甲酸溶液为流动相进行梯度洗脱,质谱分析采用电喷雾正离子多反应监测模式,基质加标工作曲线法定量。结果表明,9种非甾体类药物的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3S/N)为0.005~0.060 ng·L^(-1)。按照标准加入法进行回收试验,回收率为86.1%~107%,日内、日间精密度试验所得测定值的相对标准偏差(n=6)分别为3.0%~7.4%和3.8%~8.4%。方法用于40份实际生活污水样品的分析,结果显示生活污水中甲氧苄啶、马来酸氯苯那敏、安替比林、苯海拉明、异丙安替比林、酮洛芬和地西泮等7种化合物有检出,其中地西泮检出率为100%,安替比林的检出量最高,达117.46 ng·L^(-1)。
A method for the determination of 9 trace common nonsteroidal drugs,including trimethoprim,chlorpheniramine maleate,isopropyl antipyrine,antipyrine,phenacetin,diphenhydramine,mefenamic acid,diazepam,and ketoprofen,in domestic sewage was proposed by liquid chromatography tandem mass spectrometry(LC-MS/MS)with solid phase extraction.The sewage sample was filtered with 0.45μm fiberglass filter membrane,and 1.0 L of water sample was collected.2.5 g of disodium ethylenediaminetetraacetate(Na2EDTA)was added,shaking for 5 min.The solution was passed through HLB solid phase extraction cartridge at 10 mL·min^(-1),which was pre-activated with 5 mL of methanol and 5 mL of water,respectively.Elution was carried out with 5 mL of water and 5 mL of methanol,and the eluate was collected and blown to nearly dryness by nitrogen.The residue was reconstituted in 1.0 mL of 20%(volume fraction)methanol solution,and the solution was mixed by vortexing for 1 min,and passed through 0.2μm filter membrane.Liquid chromatography separation was performed on a BEH C18 column(100 mm×2.1 mm,1.7μm),with a mixture of acetonitrile solution containing 0.1%(volume fraction,the same below)formic acid and 0.1%formic acid solution at different volume ratios as mobile phase for gradient elution,and electrospray ion(ESI)in the positive multiple reaction monitoring(MRM)mode was adopted in MS analysis.Quantification was carried out by matrix spiked working curves.As shown by the results,linear relationships between values of the corresponding peak area and mass concentration of 9 nonsteroidal drugs were found in definite ranges,with detection limits(3S/N)in the range of 0.005-0.060 ng·L^(-1).Recovery test was carried out according to the standard addition method,giving results in the range of 86.1%-107%,with RSDs(n=6)of the determined values in the range of 3.0%-7.4%for intra-day precision test and 3.8%-8.4%for inter-day precision test,respectively.This method was used for the analysis of 40 actual domestic sewage samples,and it was shown that 7 compo
作者
傅容
陈晓红
FU Rong;CHEN Xiaohong(West China College of Public Health,Sichuan University,Chengdu 610044,China;Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals,Ningbo Municipal Center for Disease Control and Prevention,Ningbo 315010,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第3期303-309,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
宁波市医学重点学科建设计划(2022B18)。
关键词
非甾体类药物
液相色谱-串联质谱法
生活污水
固相萃取
nonsteroidal drug
liquid chromatography tandem mass spectrometry
domestic sewage
solid phase extraction
