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采用改良的 QuEChERS 结合超高效液相色谱-串联质谱法同时分析水果和蔬菜中高氯酸盐 (ClO) 和溴酸盐 (BrO) 的新方法。

A novel approach for simultaneous analysis of perchlorate (ClO) and bromate (BrO) in fruits and vegetables using modified QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry.

机构信息

School of Food Science and Engineering, South China University of Technology, Guangzhou 510640, China.

School of Food Science and Engineering, South China University of Technology, Guangzhou 510640, China.

出版信息

Food Chem. 2019 Jan 1;270:196-203. doi: 10.1016/j.foodchem.2018.07.091. Epub 2018 Jul 17.

Abstract

Perchlorate (ClO) and bromate (BrO) are mainly determined by ion chromatography methods. The present work aims to develop a modified QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous analysis of ClO and BrO in fruits and vegetables including cherry tomato, strawberry, tomato, potato, lettuce and pakchoi. Two target inorganic anions were separated on a Diamonsil C18(2) column by gradient elution, scanned in ESI negative mode and detected under multiple reactions monitoring (MRM). Limit of detection (LOD) and method limit of quantification (MLOQ), matrix effect, accuracy and precision of the developed method were investigated. Results were linear in their concentration ranges, with coefficients of determination (r) bigger than 0.999. LODs for ClO and BrO were 0.1 μg/L and 0.5 μg/L, respectively. The validated method provided sufficient selectivity, sensitivity and accuracy to screen for ClO and BrO with ignorable matrix effects. Recoveries for different kinds of negative samples at 3 spiked levels were between 82.0% and 99.5%. Both intraday-precision and interday-precision were satisfactory, showing RSDr values in the range of 2.1-7.1% and RSD values in the range of 7.2-10.8%. The proposed method was successfully applied to determine target inorganic anions in several fruits and vegetables. Perchlorate was detected in 12 vegetable samples with the concentrations ranged from 21 μg/kg to 162 μg/kg. Results indicated that there was wide ClO contamination in vegetables, confirming its urgency for monitoring harmful inorganic anions in our daily consumed vegetables.

摘要

高氯酸盐(ClO)和溴酸盐(BrO)主要通过离子色谱法测定。本工作旨在建立一种改良的 QuEChERS 与超高效液相色谱-串联质谱法(UPLC-MS/MS)相结合的方法,用于同时分析樱桃番茄、草莓、番茄、土豆、生菜和白菜等果蔬中的 ClO 和 BrO。两种目标无机阴离子在 Diamonsil C18(2)柱上通过梯度洗脱分离,在电喷雾负离子模式下扫描,在多重反应监测(MRM)下检测。对所建立方法的检测限(LOD)和定量限(MLOQ)、基质效应、准确度和精密度进行了研究。结果在其浓度范围内呈线性,相关系数(r)均大于 0.999。ClO 和 BrO 的检出限(LOD)分别为 0.1μg/L 和 0.5μg/L。该验证方法具有足够的选择性、灵敏度和准确度,可用于筛选具有可忽略基质效应的 ClO 和 BrO。在 3 个加标水平下,不同阴性样品的回收率在 82.0%至 99.5%之间。日内精密度和日间精密度均令人满意,RSDr 值在 2.1%至 7.1%范围内,RSD 值在 7.2%至 10.8%范围内。该方法成功应用于几种水果和蔬菜中目标无机阴离子的测定。在 12 个蔬菜样品中检测到高氯酸盐,浓度范围为 21μg/kg 至 162μg/kg。结果表明,蔬菜中 ClO 污染广泛,证实了对日常食用蔬菜中有害无机阴离子进行监测的紧迫性。

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