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采用 QuEChERS 法和液相色谱-串联质谱法测定人乳中的四种对羟基苯甲酸酯和双酚 A、F 和 S

Determination of four parabens and bisphenols A, F and S in human breast milk using QuEChERS and liquid chromatography coupled to mass spectrometry.

机构信息

Public Health Laboratory of Valencia, Av. Catalunya, 21, 46020, Valencia, Spain; Department of Analytical Chemistry, University of Valencia, Doctor Moliner 50, 46100 Burjassot, Spain.

Foundation for the Promotion of Health and Biomedical Research in the Valencia Region, FISABIO-Public Health, Av. Catalunya 21, 46020, Valencia, Spain.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 May 1;1114-1115:154-166. doi: 10.1016/j.jchromb.2019.03.004. Epub 2019 Mar 7.

Abstract

For the first time, a multiresidue, sensitive and high throughput method for determination of bisphenol A, F and S and 4 parabens (methyl paraben, ethyl paraben, propyl paraben and butyl paraben) in human breast milk was developed. The proposed method includes an extraction and clean-up procedure based on QuEChERS methodology followed by liquid chromatography coupled to triple quadrupole mass spectrometry determination. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for mass detection. During the method validation the recoveries varied between 83 and 115% with a precision lower than 20% for all analytes using spiked levels from 0.1 to 50 ng mL. The LOQ was 0.10 ng mL for most of the analytes. The proposed method was successfully applied for the determination of these compounds in 10 breast milk samples from volunteer lactating mothers from the Valencian region (Spain). Among parabens, methyl paraben presented the highest detection frequency (80%) with a concentration range of 0.11-7.00 ng mL, while bisphenol A was detected more frequently than BPF and BPS (80% of detection frequency) with concentrations ranging from 0.13 to 1.62 ng mL.

摘要

首次建立了一种多残留、灵敏且高通量的方法,用于测定人乳中的双酚 A、F 和 S 以及 4 种对羟基苯甲酸酯(甲基对羟基苯甲酸酯、乙基对羟基苯甲酸酯、丙基对羟基苯甲酸酯和丁基对羟基苯甲酸酯)。该方法包括基于 QuEChERS 方法的提取和净化程序,随后进行液相色谱-串联三重四极杆质谱测定。采用负离子大气压化学电离,在选择反应监测模式下进行质谱检测。在方法验证过程中,所有分析物的回收率在 83%至 115%之间变化,加标水平为 0.1 至 50ng/mL 时,精密度均低于 20%。大多数分析物的 LOQ 为 0.10ng/mL。该方法成功应用于测定来自西班牙瓦伦西亚地区自愿哺乳期母亲的 10 个人乳样本中的这些化合物。在对羟基苯甲酸酯中,甲基对羟基苯甲酸酯的检出频率最高(80%),浓度范围为 0.11-7.00ng/mL,而双酚 A 的检出频率高于 BPF 和 BPS(80%的检出频率),浓度范围为 0.13-1.62ng/mL。

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