Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

LIN Qiang; WANG Jian; LI Jing-jing; SU Dong-xia; LI Mei-li; WANG Jia; NIU Yu-min

doi:10.12452/j.fxcsxb.24022901

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Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

Scientific Papers | 更新时间：2024-08-08

- Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 8, Pages: 1235-1241(2024)
- 作者机构：
  
  1.北京市延庆区疾病预防控制中心，北京 102100
  2.北京市延庆区永宁社区卫生服务中心，北京 102100
  3.北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室，北京 100013
  4.首都医科大学公共卫生学院，北京 100069
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.24022901
  CLC： O657.7;X132
- Published：15 August 2024，
  
  Received：29 February 2024，
  
  Revised：07 April 2024，
- 稿件说明：
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林强,王健,李晶晶,苏东霞,李美丽,王佳,牛宇敏.超高效液相色谱-串联质谱法测定血清中26种有机磷酸酯类化合物[J].分析测试学报,2024,43(08):1235-1241.

LIN Qiang,WANG Jian,LI Jing-jing,SU Dong-xia,LI Mei-li,WANG Jia,NIU Yu-min.Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(08):1235-1241.
林强,王健,李晶晶,苏东霞,李美丽,王佳,牛宇敏.超高效液相色谱-串联质谱法测定血清中26种有机磷酸酯类化合物[J].分析测试学报,2024,43(08):1235-1241. DOI： 10.12452/j.fxcsxb.24022901.

LIN Qiang,WANG Jian,LI Jing-jing,SU Dong-xia,LI Mei-li,WANG Jia,NIU Yu-min.Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(08):1235-1241. DOI： 10.12452/j.fxcsxb.24022901.

摘要

采用超高效液相色谱-串联质谱（UPLC-MS/MS）建立了血清中26种有机磷酸酯类化合物的检测方法。血清样本经乙腈沉淀蛋白后，通过HMR固相萃取小柱净化，净化液氮吹至近干，甲醇复溶后上机检测。以5 mmol/L乙酸铵水溶液和甲醇为流动相，使用C

色谱柱分离目标物，质谱采用电喷雾离子源（正离子模式），以多反应监测模式检测，稳定同位素内标法定量。结果表明，26种有机磷酸酯类化合物在相应质量浓度范围内线性关系良好（

＞0.997），检出限为0.024～0.146 ng/mL，定量下限为0.079～0.483 ng/mL。血清样本的加标回收率为85.7%～115%，相对标准偏差为4.5%～12%。使用该方法检测实际血清样本，检出2种有机磷酸酯类化合物。该方法操作简便、灵敏度高、精密度好，适用于大批量血清样本中有机磷酸酯类化合物的痕量检测。

Abstract

A detection method for 26 organophosphate esters in serum was established using ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. After precipitation of protein with acetonitrile，the serum sample was purified by HMR solid phase extraction column，and the purified liquid nitrogen was blown to near dryness. After redissolving in methanol，it was detected on the machine. With 5 mmol/L ammonium acetate aqueous solution and methanol as mobile phase，the target substances were separated by C

chromatographic column. The mass spectrum was detected by electrospray ion source（positive ion mode），multi reaction monitoring mode and stable isotope internal standard method. The results showed that the 26 organophosphate esters had a good linear relationship within the corresponding mass concentration range（

0.997），with detection limits of 0.024 ng/mL to 0.146 ng/mL and quantification limits of 0.079 ng/mL to 0.483 ng/mL. The spiked recoveries of serum sample is 85.7% to 115%，with relative standard deviations of 4.5% to 12%. This method was used to detect actual serum samples，and two types of organophosphate esters were detected. This method is easy to operate，highly s

ensitive，and has good precision，which is suitable for the trace detection of organophosphate esters in large quantities of serum samples.

关键词

有机磷酸酯血清超高效液相色谱-串联质谱法固相萃取

Keywords

organophosphate estersserumultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）solid phase extraction

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