Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

ZHANG Hai-chao; WANG Jing; JIA Hai-tao; LI Wei; AI Lian-feng; KANG Wei-jun

doi:10.3969/j.issn.1004-4957.2021.07.017

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Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods

- Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 40, Issue 7, Pages: 1086-1090(2021)
- 作者机构：
  
  1.石家庄海关技术中心，河北石家庄 050051
  2.河北医科大学公共卫生学院，河北石家庄 050017
- 作者简介：
- 基金信息：
- DOI：10.3969/j.issn.1004-4957.2021.07.017
  CLC：
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张海超,王敬,贾海涛等.固相萃取/超高效液相色谱－串联质谱法测定香辛调料中的曲托喹酚[J].分析测试学报,2021,40(07):1086-1090.

ZHANG Hai-chao,WANG Jing,JIA Hai-tao,et al.Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(07):1086-1090.
张海超,王敬,贾海涛等.固相萃取/超高效液相色谱－串联质谱法测定香辛调料中的曲托喹酚[J].分析测试学报,2021,40(07):1086-1090. DOI： 10.3969/j.issn.1004-4957.2021.07.017.

ZHANG Hai-chao,WANG Jing,JIA Hai-tao,et al.Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(07):1086-1090. DOI： 10.3969/j.issn.1004-4957.2021.07.017.

摘要

采用MCX固相萃取柱净化，以超高效液相色谱－串联质谱（UPLC－MS/MS）法建立了香辛调料中曲托喹酚的测定方法。样品采用0.2%酸性乙醇提取，经MCX柱净化浓缩后，在ACQUITY BEH C,18,色谱柱上以乙腈和0.1%甲酸水溶液为流动相梯度洗脱，UPLC－MS/MS以MRM方式进行定量分析。结果表明，曲托喹酚在0.1～50 ng/mL范围内线性关系良好，相关系数（,r,）大于0.998，方法的检出限（LOD）为0.2 μg/kg，定量下限（LOQ）为0.5 μg/kg。化合物在不同基质的4个加标水平（0.5、2、10、100 μg/kg）下的回收率为74.5%～98.8%，相对标准偏差（RSD）为3.1%～9.1%。该方法灵敏、准确、可靠，可用于香辛调料中曲托喹酚的测定。

Abstract

An ultra-performance liquid chromatography－tandem mass spectrometric（UPLC－MS/MS） method was developed for the determination of tretoquinol in pungent spice with MCX solid-phase extraction（SPE） purification. The samples were extracted with 0.2% acid ethanol， purified with a MCX column， and quantified by UPLC－MS/MS in MRM mode after gradient elution on an ACQUITY BEH C,18, column with acetonitrile and 0.1% formic acid solution as mobile phase. The results showed that the calibration curves were linear in the range of 0.1－50 ng/mL with correlation coefficients（,r,） more than 0.998. The limits of detection （LODs） were 0.2 μg/kg and the limits of quantitation （LOQs） were 0.5 μg/kg. The average recoveries of tretoquinol at four different spiked levels （0.5， 2， 10， 100 μg/kg） ranged from 74.5% to 98.8%，with relative standard deviations（RSD） of 3.1%－9.1%. The proposed method is sensitive， accurate and reliable， and could be used for the determination of tretoquinol in pungent spice.

关键词

曲托喹酚固相萃取超高效液相色谱－串联质谱（UPLC－MS/MS）香辛调料

Keywords

tretoquinolsolid-phase extractionultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）pungent spice

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