利用SBSE-GC-MS技术快速检测自来水中多环芳烃及塑化剂  

Rapid determination of polycyclic aromatic hydrocarbons and phthalates in tap water by SBSE combined with GC-MS

作　　者：田春霞 盛燕燕 姚燕红 赵永信[1] 张念华[1] Tian Chunxia;Sheng Yanyan;Yao Yanhong;Zhao Yongxin;Zhang Nianhua(Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou 310051,China)

机构地区：[1]浙江省疾病预防控制中心,杭州310051

出　　处：《卫生研究》2024年第4期646-655,共10页Journal of Hygiene Research

基　　金：浙江省疾病预防控制中心科技英才孵育项目(No.2023-A-03);浙江省医药卫生科技计划项目(No.2024KY908)。

摘　　要：目的 以搅拌棒吸附萃取为样品前处理技术,结合气相色谱-质谱联用法,建立同时检测自来水中16种多环芳烃和16种塑化剂的快速检测方法。方法 老化后的乙二醇极性搅拌棒直接放入装有50 mL自来水的样品瓶中,同时将聚二甲基硅氧烷搅拌棒固定在样品瓶的瓶壁上,浸入液体中。向样品瓶中添加5%(W/V)氯化钠和5%甲醇,室温下搅拌提取2 h。取出2个搅拌棒,擦干表面水分并晾干,放入热解吸玻璃管中待测。程序升温热脱附温度至275℃,保持该温度时间15 min,冷阱温度-40℃对热脱附后的物质进行冷阱捕集,最后全部进入气相色谱-质谱仪进行分离检测。结果 16种多环芳烃和16种塑化剂在200~2000 ng/L范围内响应峰面积与其浓度呈良好的线性关系(R^(2)>0.986),检出限为1.13~121 ng/L,200及2000 ng/L 2个添加浓度水平的平均回收率为62.5%~98.4%,相对标准偏差(n=5)为3.5%~25.3%。结论 建立的搅拌棒吸附萃取结合气相色谱-质谱联用法简单,操作便捷,提取和分析时间较短,背景值更容易控制,可以实现实验室的高通量快速检测。OBJECTIVE To develop a method which is used for rapid determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) and 16 kinds of phthalates(PAEs) in tap water by stirring rod adsorption extraction(SBSE) combined with gas chromatography-mass spectrometry(GC-MS).METHODS The twister mixing rod coated with polydimethylsiloxane(PDMS) and ethylene glycol-polydimethylsiloxane(EG-silicone) was used to enrich analyte from 50 mL tap water.The twister mixing rod coated with EG-silicone was directly placed into the sample bottle containing 50 mL of tap water,while fixing the PDMS stir bar on the inner wall of the sample bottle and immersing it in the liquid.Add 5%(W/V) sodium chloride to the sample bottle,followed by adding 5% methanol.Stir at room temperature for 2 hours for extraction.Next,remove the mixing stick and dry its surface.The pre-prepared SBSE was analyzed by TD-GC/MS,with the optimized thermal desorption conditions:desorption temperature 275 ℃,desorption time 15 min,cryofocusing temperature-40 ℃.RESULTS Regression equations revealed acceptable linearity(correlation coefficients >0.986) across the working-standard range from 200-2000 ng/L for the 32 analytes.The limits of detection(LODs)were further evaluated were from 1.13-121 ng/L.With the optimized pretreatment method,the spiked recoveries of tap samples(200 and 2000 ng/L)were in the range of 62.5%-98.4% with the relative standard deviations(RSDs) of 3.5%-25.3%.CONCLUSION The established method can realize the rapid detection of high throughput in the laboratory,it is simple,convenient to operate,and the extraction and analysis time is short.

关 键 词：搅拌棒吸附萃取 多环芳烃 塑化剂 水 气相色谱-质谱 

分 类 号：O657[理学—分析化学]