摘要
开发了一种利用高效液相色谱-串联质谱法同时测定学生用品中全氟己烷磺酸、全氟辛酸和全氟辛烷磺酸含量。样品以甲醇为溶剂,在超声波清洗器中常温提取,然后离心,最后移取4 mL上清液到离心管中,用缓慢的氮气流吹至1 mL,经滤膜净化后装入进样小瓶,经选择离子确认,以外标法定量。3种全氟化合物的质量浓度在2~100μg/L范围内与色谱峰面积的线性关系良好,检出限为0.003~0.010 mg/kg,定量限为0.003~0.030 mg/kg。对阴性文具样品进行低、中、高浓度水平的加标回收试验,回收率为86.0%~101.8%,测定结果的相对标准偏差均小于5.0%(n=7)。该方法可以满足学生用品中3种全氟化合物的测试需求。
A method for simultaneous detection of Perfluorohexane sulfonic acid,perfluorooctanoic acid,and perfluorooctane sulfonic acid in school supplies by high performance liquid chromatography-tandem mass spectrometry(HPLC/MS-MS)was developed.The samples were extracted at room temperature using methanol as the solvent in an ultrasonic cleaner,and then centrifuged.Finally,4 mL of the supernatant was transferred to a centrifuge tube and blown to 1 mL with a slow nitrogen flow.After purification through a filter membrane,it was loaded into an injection vial and confirmed by ion selection.Quantification was performed using an external standard method.The linear relationships between the mass concentration of three perfluorinated compounds and the chromatographic peak areas were good within the range of 2-100μg/L,and the detection limits were 0.003-0.010 mg/kg,the limit of quantification was 0.003-0.030 mg/kg.Low,medium,and high concentration spiked recovery tests were conducted on negative stationery samples,with recovery rates of 86.0%-101.8%.The relative standard deviations of the measurement results were all less than 5.0%(n=7).This method can meet the testing needs simultaneous detection of three perfluorinated compounds in school supplies.
作者
张慧
马红青
蒋莹
ZHANG Hui;Ma Hongqing;JIANG Ying(Institute of Quality Inspection of Light Industry&Chemical products,Shanghai Institute of quality Inspection and Technical Research,Shanghai 201114,China)
出处
《化学分析计量》
CAS
2024年第12期41-45,共5页
Chemical Analysis And Meterage
基金
上海市市场监督管理局科技项目(2024-24)。
关键词
高效液相色谱串联质谱法
学生文具
全氟化合物
新污染物
持久性
high performance liquid chromatography tandem mass spectrometry
school supplies
perfluorinated compound
new pollutants
persistence
