高效液相色谱-串联质谱法测定医用口罩中8种全氟化合物  

Determination of 8 Perfluorinated Compounds in Medical Mask by HPLC-MS/MS

作　　者：石刚 凌婷 李慧玲 张娜 孙世元 蒋付良 SHI Gang;LING Ting;LI Huiling;ZHANG Na;SUN Shiyuan;JIANG Fuliang(Jiaxing Institute for Food Drug and Product Quality Control,Jiaxing 314001;National Quality Inspection Center of Garment Accessorier(Zhe Jiang),Jiaxing 314050)

机构地区：[1]嘉兴市食品药品与产品质量检验检测院,浙江嘉兴314001 [2]国家服装辅料产品质量检验检测中心(浙江),浙江嘉兴314050

出　　处：《分析科学学报》2024年第1期50-56,共7页Journal of Analytical Science

基　　金：浙江省市场监督管理局科研计划项目(2021000010)。

摘　　要：采用高效液相色谱-串联质谱(LC-MS/MS)技术建立了医用口罩中全氟辛酸、全氟辛烷磺酸钾、全氟十一酸、全氟十二酸、全氟辛烷磺酸胺、全氟十三酸、全氟十四酸、N-乙基全氟辛烷磺酸胺8种全氟化合物的测定方法。样品以甲醇为溶剂,超声提取,采用C_(18)(150 mm×2.1 mm,5μm)色谱柱分离,流动相为甲醇和乙酸铵,梯度洗脱,多反应监测(MRM)模式进行分析检测,外标法定量。结果表明:8种全氟化合物的定量限(LOQ,以信噪比>10计)为0.50~1.58μg/kg,在0.5~10μg/L时标准曲线线性关系良好(r>0.9979),样品加标回收率为98.4%~102.3%,相对标准偏差为1.55%~7.44%。该方法前处理简单,回收率高,精密度好,适用于医用口罩中全氟化合物的检测。A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the determination of 8 perfluorinated compounds(PFCs) in medical mask,including pentadecafluorooctanoic acid(PFOA),perfluorooctanesulfonic acid potassium salt(PFOS(K)),perfluoroundecanoic acid(PFUdA),perfluorododecanoic acid(PFDoA),perfluorooctanesulfonamide(PFOSA),perfluorotridecanoic acid(PFTrDA),perfluorotetradecanoic acid(PFTeDA),sulfluramid(N-EtPFOSA).Samples were extracted with methanol through ultrasonic method.The target ingredients were separated on a C_(18) column(150 mm × 2.1 mm,5 μm) using a mixture of methanol-ammonium acetate system as mobile phase by gradient elution.The 8 perfluorinated compounds were analyzed by MS under multiple reaction monitoring mode(MRM) and quantified by the external standard method.The results showed that the limits of quantitation of 8 perfluorinated compounds were between 0.50 and 1.58 μg/kg.The calibration curve of PFCs presented good linearity with the linearity range of 0.5-10.00 μg/L.The recoveries of 8 PFCs were in the range of 98.4%-102.3% with relative standard deviations(RSDs,n=6) of 1.55%-7.44%.The method was simple,accurate and sensitive,and was suitable for the determination of PFCs in medical mask.

关 键 词：医用口罩 全氟化合物 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]