Determination of 7 Phenolic Environmental Hormones in Citrus by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry

LIU Fang; GONG Fang; QING Jiang; YANG Chu-yue; MENG Tao-yu; DING Li

doi:10.19969/j.fxcsxb.21031702

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Determination of 7 Phenolic Environmental Hormones in Citrus by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-02-13

- Determination of 7 Phenolic Environmental Hormones in Citrus by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 40, Issue 12, Pages: 1765-1771(2021)
- 作者机构：
  
  1.长沙理工大学化学与食品工程学院，湖南长沙 410000
  2.长沙和合医学检验实验室有限公司，湖南长沙 410000
  3.上海海关工业品与原材料检测技术中心，上海 200135
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21031702
  CLC：
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刘芳,龚芳,清江等.QuEChERS/高效液相色谱－串联质谱法测定柑橘中7种酚类环境激素[J].分析测试学报,2021,40(12):1765-1771.

LIU Fang,GONG Fang,QING Jiang,et al.Determination of 7 Phenolic Environmental Hormones in Citrus by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1765-1771.
刘芳,龚芳,清江等.QuEChERS/高效液相色谱－串联质谱法测定柑橘中7种酚类环境激素[J].分析测试学报,2021,40(12):1765-1771. DOI： 10.19969/j.fxcsxb.21031702.

LIU Fang,GONG Fang,QING Jiang,et al.Determination of 7 Phenolic Environmental Hormones in Citrus by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1765-1771. DOI： 10.19969/j.fxcsxb.21031702.

摘要

建立了QuEChERS/高效液相色谱－串联质谱（QuEChERS/HPLC－MS/MS）同时检测柑橘中7种酚类环境激素的分析方法。柑橘样品均质粉碎后采用乙腈（含0.1%甲酸）超声提取，氯化钠盐析，经N-丙基乙二胺（PSA）+C,18,粉末吸附剂净化，目标化合物经Waters ACQUITY UPLC BEH C,18,柱（50 mm × 2.1 mm，1.7 μm）分离，以水（含0.5 mmol/L乙酸铵）和甲醇为流动相进行梯度洗脱。考察了不同提取溶剂、提取时间、提取溶剂体积、吸附剂种类和用量对目标化合物回收率的影响。结果表明：在最佳条件下，双酚A（BPA）、壬基酚（NP）、双酚F（BPF）在0.5～100 μg/L范围内线性关系良好，双酚B（BPB）、双酚S（BPS）、4-,n,-壬基酚（4-,n,-NP）、4-,n,-辛基酚（4-,n,-OP）在0.2～100 μg/L范围内线性关系良好，相关系数（,r,2,）均不小于0.994 1，检出限（LOD）为0.2～0.5 μg/L，定量下限（LOQ）为0.5～1.5 μg/L。在10、250、500 μg/kg 3个加标水平下，目标化合物的回收率为88.5%～109%，相对标准偏差（RSD）为1.2%～9.0%。应用该方法对市售的8种柑橘样品进行检测，BPA在7种柑橘中均检出，4-,n,-OP在5种柑橘中检出，NP和4-,n,-NP在3种柑橘中检出，BPB在1种柑橘中检出，BPF、BPS在所有样品中均未检出。该方法操作简单、快速灵敏、定量准确、精密度高，适用于柑橘中7种酚类环境激素的测定。

Abstract

A QuEChERS/high performance liquid chromatography－tandem mass spectrometry（QuEChERS/HPLC－MS/MS） was established for the simultaneous detection of seven phenolic environmental hormones in citrus．Effects of different extraction solvents，extraction time，extraction solvent volume and adsorbent types on the extraction efficiency for target compounds were compared．The samples were ultrasonically extracted twice with acetonitrile containing 0.1% formic acid after homogenization，and then purified by modified QuEChERS method with 50 mg PSA + 50 mg C,18,．The target compounds were separated on a Waters ACQUITY UPLC BEH C,18, column（50 mm × 2.1 mm，1.7 μm） by gradient elution，with water containing 0.5 mmol/L ammonium acetate and methanol as the mobile phases at a flow rate of 0.2 mL/min and a column temperature of 40 ℃．The mass spectra were recorded by negative electrospray ionization under the multiple reaction monitoring（MRM） mode．External standard method was used for the quantitative analysis．Under the optimized conditions，bisphenol A（BPA），nonylphenol（NP），bisphenol F（BPF） showed good linear relationships within the range of 0.5－100 μg/L，while bisphenol B（BPB），bisphenol S（BPS），,n,-nonylphenol（4-,n,-NP），,n,-octylphenol（4-,n,-OP） exhibited good linear relationships within 0.2－100 μg/L．The correlation coefficients（,r,2,） were not less than 0.994 1. The detection limits（LOD）and the quantitation limits（LOQ）of the method were in the ranges of 0.2－0.5 μg/L and 0.5－1.5 μg/L，respectively．At the three spiked levels of 10，250 and 500 μg/kg，the average recoveries for the target compounds ranged from 88.5% to 109%，with the relative standard deviations（RSD）of 1.2%－9.0%．The method was applied to the detection of 8 commercially available citrus samples．BPA was detected in 7 kinds of citrus，4-,n,-OP was detected in 5 kinds of citrus，NP and 4-,n,-NP were detected in 3 types of citrus，BPB was detected in 1 type of citrus，and BPF and BPS were not detected in all samples．The above results indicate that bisphenol environmental hormones are commonly found in commercially available fruits and need to be paid attention to．This method was simple to operate，rapid，sensitive，accurate and highly precise．It was suitable for the determination of 7 bisphenol environmental hormones in citrus．

关键词

高效液相色谱－串联质谱分散固相萃取环境激素柑橘

Keywords

high performance liquid chromatography－tandem mass spectrometryQuEChERSenvironmental hormonescitrus

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