Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography－Tandem Mass Spectrometry

WANG Tao; ZHANG Hong; ZHOU Han-lin; LIN Jie; TONG Ping; BEN Yu-jie; WANG Yao-qiang; HAN Yong-he; ZHANG Yong; LI Jia-bing

doi:10.19969/j.fxcsxb.23032803

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Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-07-12

- Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 7, Pages: 825-832(2023)
- 作者机构：
  
  1.福建师范大学环境与资源学院，碳中和现代产业学院，福建福州 350117
  2.福建省污染控制与资源循环利用重点实验室，福建福州 350117
  3.福州大学福建省高校测试中心，福建福州 350116
  4.南方科技大学环境科学与工程学院，广东深圳 518055
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23032803
  CLC：
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王涛,张虹,周寒琳等.固相萃取/高效液相色谱－串联质谱法同时测定土壤中12种有机磷酸酯[J].分析测试学报,2023,42(07):825-832.

WANG Tao,ZHANG Hong,ZHOU Han-lin,et al.Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):825-832.
王涛,张虹,周寒琳等.固相萃取/高效液相色谱－串联质谱法同时测定土壤中12种有机磷酸酯[J].分析测试学报,2023,42(07):825-832. DOI： 10.19969/j.fxcsxb.23032803.

WANG Tao,ZHANG Hong,ZHOU Han-lin,et al.Simultaneous Determination of 12 Organophosphate Esters in Soil by Solid Phase Extraction/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):825-832. DOI： 10.19969/j.fxcsxb.23032803.

摘要

采用固相萃取结合高效液相色谱－串联质谱（HPLC－MS/MS）技术，建立了同时测定土壤中12种有机磷酸酯（OPEs）的方法。土壤样品经冷冻干燥、过筛后，加入丙酮－正己烷（1∶1，体积比）超声提取，经CNWBOND Florisil SPE小柱净化后，进行HPLC－MS/MS分析，采用内标法定量。12种OPEs在0.1 ~ 100 μg/L质量浓度范围内线性良好，相关系数（,r,2,）均大于0.999，检出限为0.004 ~ 0.162 ng/g。在低、中、高3种加标水平下，平均加标回收率为67.0% ~ 128%，相对标准偏差为1.5% ~ 9.9%。利用该方法对20份土壤样本进行检测，12种目标化合物均有检出，OPEs总含量为5.36 ~ 55.2 ng/g（干重），平均值为23.7 ng/g（干重），中位数为25.0 ng/g（干重）。该方法灵敏度高，准确度和精密度良好，适用于土壤样品中OPEs的测定。

Abstract

An effective analytical method was established for the determination of 12 organophosphate esters（OPEs） in soil by solid phase extraction coupled with high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） in this paper．After freeze-drying and sieving，the soil samples were ultrasonically extracted with acetone－hexane（1∶1，by volume），then purified with a CNWBOND Florisil SPE cartridge，and finally analyzed by HPLC－MS/MS．The internal standard method was used for quantification．There were good linear relationships for 12 OPEs in the concentration range of 0.1－100 μg/L，with correlation coefficients（,r,2,） greater than 0.999 and detection limits of 0.004－0.162 ng/g．The average recoveries at low，medium and high three spiked levels ranged from 67.0% to 128%，with relative standard deviations of 1.5%－9.9%．12 OPEs were detected simultaneously in 20 soil samples by the method established．All target compounds were detected with a total content of OPEs ranging from 5.36 to 55.2 ng/g（dry weight），the mean value of 23.7 ng/g（dry weight） and the median value of 25.0 ng/g（dry weight）．This method is suitable for the determination of OPEs in soil samples with sensitive and reliable results.

关键词

有机磷酸酯土壤固相萃取高效液相色谱－串联质谱法

Keywords

organophosphate esterssoilsolid phase extractionhigh performance liquid chromatography－tandem mass spectrometry

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