超高效液相色谱-串联质谱法测定环境水体中23种内分泌干扰物的含量  

Determination of 23 Endocrine Disrupting Chemicals in Environmental Water Body by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：杨超 尹明明 王美飞 刘景龙 YANG Chao;YIN Mingming;WANG Meifei;LIU Jinglong(Nanjing Environmental Monitoring Center of Jiangsu Province,Nanjing 210013,China)

机构地区：[1]江苏省南京环境监测中心,南京210013

出　　处：《理化检验（化学分册）》2024年第9期905-914,共10页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省南京环境监测中心科研项目(202204)。

摘　　要：提出了超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定环境水体中23种内分泌干扰物(EDCs)含量的方法。用6 mol·L^(-1)盐酸溶液调节水样p H约为2.0,取100 mL水样置于250 mL分液漏斗中,加入3 g氯化钠,振荡,加入30 mL体积比1∶1的乙酸乙酯-二氯甲烷混合溶液,振荡5 min,静置,下层有机相经无水硫酸钠除水,旋转蒸发近干后,加入乙腈0.2 mL,再加入2.0 mg·L^(-1)混合内标使用液10μL,用水定容至1 mL,过0.22μm再生纤维素滤膜后采用UHPLC-MS/MS测定滤液中23种EDCs的含量。以BEN C_(18)色谱柱为固定相,以不同体积比的0.05%(体积分数)氨水溶液-乙腈混合液为流动相进行梯度洗脱,质谱分析采用电喷雾离子(ESI)源,在负离子(ESI^(-))扫描模式下采用多反应监测(MRM)模式检测。结果表明,23种EDCs的质量浓度在一定范围内与对应的峰面积与内标峰面积比呈线性关系,检出限(3.143s)为0.60~1.75 ng·L^(-1);按照标准加入法进行回收试验,回收率为72.6%~107%,测定值的相对标准偏差(n=6)均小于14%;方法用于测定实际环境水体中23种EDCs的含量,结果显示在地表水中双酚AF的质量浓度最高,为27.9 ng·L^(-1),在污水及废水中普遍检出4-正壬基酚和4-特辛基酚,检出量分别为838~2 353 ng·L^(-1)和87.8~16 733 ng·L^(-1)。A method for determination of 23 endocrine disrupting chemicals(EDCs) in environmental water body by ultrahigh performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) was proposed.The pH of water sample was adjusted to about 2.0 with 6 mol · L^(-1) hydrochloric acid solution.100 mL of water sample was taken into a 250 mL-separatory funnel,and 3 g of sodium chloride was added.The mixture was shaken,and 30 mL of a mixture of ethyl acetate and dichloromethane at a volume ratio of 1∶1 was added.The mixture was shaken for 5 min and settled,and the lower organic phase was dehydrated with anhydrous sodium sulfate.The solution was rotary evaporated to near dryness,and 0.2 mL of acetonitrile and 10 μL of 2.0 mg · L^(-1) mixed internal standard solution were added.The solution was made its volume up to 1 mL with water,and passed through a 0.22 μm regenerated cellulose filter membrane.23 EDCs in the filtrate were determined by UHPLC-MS/MS.BEN C_(18) chromatographic column was used as the stationary phase and the mixed solution composed of 0.05%(volume fraction) aqueous ammonia solution and acetonitrile at different volume ratios was used as the mobile phase for gradient elution.Electrospray ion(ESI) source was used for mass spectrometry.The targets were detected by multiple reaction monitoring(MRM)mode in negative ion(ESI~-) scanning mode.As shown by the results,linear relationships between the ratios of the corresponding peak area to the internal standard peak area and mass concentrations of 23 EDCs were found in definite ranges,with detection limits(3.143s) in the range of 0.60-1.75 ng · L^(-1).Test for recovery was made by the standard addition method,giving results in the range of 72.6%-107%,with RSDs(n=6) of the determined values less than 14%.This method was used to determine 23 EDCs in actual environmental water body,and it was shown that mass concentration of bisphenol AF was the highest in surface water with 27.9 ng · L^(-1),and 4-nonylphenol and 4-tert-octylphenol were commonly detected in

关 键 词：超高效液相色谱-串联质谱法 环境水体 内分泌干扰物 

分 类 号：O657.63[理学—分析化学]