[Determination of two perfluorinated compounds in urine by liquid chromatography-tandem mass spectrometry].

X H Chen, Q L Qiu
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Abstract

Objective: To establish a method for the determination of two perfluorinated compounds in urine by liquid chromatography-tandem mass spectrometry. Methods: In November 2022, urine samples were extracted by acidic methanol, purified by WAX solid phase extraction column, and eluted with methanol water, then Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used with 1.0 mmol/L ammonium acetate solution and methanol as mobile phase. The gradient elution was carried out, the detection was carried out by electrospray negative ion multiple response monitoring (MRM) mode, and the quantitative method was internal standard method. Results: Perfluorooctanoic acid and perfluorooctane sulfonic acid had a good linear relationship in the concentration range of 0.5-50.0 μg/L, and the correlation coefficient was >0.999. The limit of detection was 0.017 μg/L, and the limit of quantitation was 0.005 μg/L. The average recoveries were 96.3% and 101.8%, respectively. Days of precision were 3.5%-6.2% and 3.1%-7.4%, respectively, daytime precision were 4.3%-6.8% and 4.7%-8.1%, respectively. Conclusion: The established method of liquid chromatography-tandem mass spectrometry is high sensitivity and accuracy, and is suitable for the determination of perfluorooctanoic acid and perfluorooctane sulfonic acid in human urine.

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[利用液相色谱-串联质谱法测定尿液中的两种全氟化合物]。
目的:建立一种利用液相色谱-串联质谱法测定尿液中两种全氟化合物的方法:建立一种利用液相色谱-串联质谱法测定尿液中两种全氟化合物的方法。方法: 2022 年 11 月,用酸性甲醇提取尿液样本:2022年11月,尿样经酸性甲醇提取,WAX固相萃取柱净化,甲醇水洗脱,Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以1.0 mmol/L乙酸铵溶液和甲醇为流动相进行梯度洗脱,采用电喷雾离子源正离子多反应监测模式进行检测。采用梯度洗脱,电喷雾负离子多反应监测(MRM)模式检测,内标法定量。结果表明全氟辛酸与全氟辛烷磺酸在0.5~50.0 μg/L浓度范围内线性关系良好,相关系数大于0.999。检出限为 0.017 μg/L,定量限为 0.005 μg/L。平均回收率分别为 96.3% 和 101.8%。日精密度分别为 3.5%-6.2% 和 3.1%-7.4% ,日间精密度分别为 4.3%-6.8% 和 4.7%-8.1% 。结论所建立的液相色谱-串联质谱法灵敏度高、准确度高,适用于人体尿液中全氟辛酸和全氟辛烷磺酸的测定。
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来源期刊
中华劳动卫生职业病杂志
中华劳动卫生职业病杂志 Medicine-Medicine (all)
CiteScore
1.00
自引率
0.00%
发文量
9764
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