Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography－Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

FAN Qing-ya; BAI Ze-fang; WANG Xue-meng; WANG Wan-hao

doi:10.19969/j.fxcsxb.22041303

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Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography－Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

Experimental Techniques and Methods | 更新时间：2023-01-04

- Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography－Tandem Mass Spectrometry with Dispersive Solid Phase Extraction
- Journal of Instrumental Analysis Vol. 41, Issue 8, Pages: 1235-1241(2022)
- 作者机构：
  
  1.信阳职业技术学院，河南信阳 464000
  2.河南同源制药有限公司，河南信阳 464000
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22041303
  CLC：
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樊轻亚,白泽方,汪学猛等.分散固相萃取/超高效液相色谱－串联质谱法测定药用狗牙花中6种生物碱[J].分析测试学报,2022,41(08):1235-1241.

FAN Qing-ya,BAI Ze-fang,WANG Xue-meng,et al.Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography－Tandem Mass Spectrometry with Dispersive Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(08):1235-1241.
樊轻亚,白泽方,汪学猛等.分散固相萃取/超高效液相色谱－串联质谱法测定药用狗牙花中6种生物碱[J].分析测试学报,2022,41(08):1235-1241. DOI： 10.19969/j.fxcsxb.22041303.

FAN Qing-ya,BAI Ze-fang,WANG Xue-meng,et al.Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography－Tandem Mass Spectrometry with Dispersive Solid Phase Extraction[J].Journal of Instrumental Analysis,2022,41(08):1235-1241. DOI： 10.19969/j.fxcsxb.22041303.

摘要

建立了分散固相萃取技术（dSPE）结合超高效液相色谱－串联质谱（UPLC－MS/MS）同时测定狗牙花中6种生物碱的方法。采用单因素实验考察了分散固相萃取各因素对狗牙花中6种生物碱萃取率的影响，确定最佳萃取条件为：以1%氨水甲醇为提取溶剂，固液比（g∶mL）为1∶20，200 mg PSA + 200 mg NH,2,为混合吸附剂。样品经分散固相萃取后，以乙腈-0.1%甲酸铵为流动相进行UPLC－MS/MS分析。6种生物碱在1～100 mg/L范围内线性关系良好，相关系数均不低于0.983 7，检出限为0.05～0.10 mg/L，定量下限为0.15～0.35 mg/L；在3个加标水平（1、10、50 mg/L）下的回收率为93.2%～98.1%，相对标准偏差（RSD）不大于2.9%。采用该方法对6个产地的狗牙花进行检测，6种生物碱的含量为0.07～0.86 mg/g，加标回收率为 91.5%～98.6%，RSD为1.1%～2.9%。结果表明，该方法准确性好，灵敏度高，操作快速简单，可满足狗牙花中生物碱的检测要求。

Abstract

An ultra high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with dispersive solid phase extraction（dSPE） was developed for the simultaneous determination of six alkaloids in Ervatamia officinalis Tsiang．Effects of the dSPE experimental conditions on the extraction efficiency for six alkaloids were investigated by single factor．The optimum conditions showed that the ratio of solid to liquid（g∶mL） was 1∶20 with 1% ammonia methanol as solvent，and the amount of PSA and NH,2, mixed adsorbent was 200 mg．After dSPE extraction，the sample was analyzed by UPLC－MS/MS with acetonitrile and 0.1% ammonium formate as mobile phases．Results showed that there were good linear relationships for six alkaloids in the range of 1－100 mg/L，with their correlation coefficients not lower than 0.983 7．The limits of detection and limits of quantitation were in the range of 0.05－0.10 mg/L and 0.15－0.35 mg/L，respectively．The recoveries at three spiked levels of 1，10 and 50 mg/L ranged from 93.2% to 98.1%，with relative standard deviations（RSDs） not more than 2.9%．The method was used for the determination of six alkaloids in the samples from 6 habitats，with their contents of 0.07－0.86 mg/g．The spiked recoveries were in the range of 91.5%－98.6%，with RSDs of 1.1%－2.9%．The method is accurate，sensitive，rapid and simple，and it could meet the requirements for detection of the alkaloids in Ervatamia officinalis Tsiang.

关键词

狗牙花生物碱分散固相萃取超高效液相色谱－串联质谱法

Keywords

Ervatamia officinalis Tsiangalkaloiddispersive solid phase extractionultra high performance liquid chromatography－tandem mass spectrometry

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