食品科学 ›› 2011, Vol. 32 ›› Issue (10): 194-198.doi: 10.7506/spkx1002-6630-201110046

• 分析检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法分析测定食用植物油中痕量δ9-四氢大麻酚

张爱芝,王全林*   

  1. 宁波市产品质量监督检验研究院
  • 出版日期:2011-05-25 发布日期:2011-04-08
  • 基金资助:
    浙江省质检系统科研计划项目(20080228)

Determination of THC in Edible Vegetable Oil by Ultra-high Performance Liquid Chrmatography-Electrospray Tandem Mass Spectrometry

ZHANG Ai-zhi,WANG Quan-lin*   

  1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315041, China
  • Online:2011-05-25 Published:2011-04-08

摘要: 以电喷雾离子源(ESI)为电离源,在负离子采集模式下建立食用植物油中δ9四氢大麻酚(δ9-THC)超高效液相色谱-质谱/质谱(UPLC-MS/MS)检测方法。实验以甲醇为提取剂,经中性氧化铝固相萃取柱净化、Waters ACQUITYTM UPLC BEH-C18(2.1mm×100mm,1.7μm)色谱柱分离后以UPLC-MS/MS多反应监测模式进行分析。方法检出限和定量限分别为0.15μg/kg和0.45μg/kg。实验以δ9-氘代四氢大麻酚(δ9-THC-D3)为内标物,采用内标法定量。3个添加水平,平均回收率为68.0%~110.0%,相对标准偏差为8.8%~18.1%。本方法能够满足食用植物油中δ9-四氢大麻酚痕量检测的要求。

关键词: 食用植物油, 四氢大麻酚, 超高效液相色谱一质谱/质谱, 负离子模式

Abstract: A determination method for δ9-tetrahydrocannabinol (THC) in edible vegetable oil was developed on the basis of ultra-high performance liquid chrmatography-electrospray tandem mass spectrometry (UPLC-MS/MS) under negative ion mode using electrospray ionization (ESI) source. THC was extracted with methanol and then purified by LC-alumina-N solid phase extraction column. Qualitative and quantitative analysis were carried out for the analyte under a MRM mode after THC was separated on Waters ACQUITY UPLCTM BEH C18 (1.7 μm, 2.1 mm×100 mm) column. The limit of detection (LOD) of the developed method was 0.15 μg/kg and the limit of quantification (LOQ) was 0.45 μg/kg for THC. Quantitative analysis was corrected by internal standard method using delta 9-THC-D3 as internal standard. Average recovery rate of THC varied from 68.0%-110.0% with relative standard deviation ranging from 8.8%-18.1% at three spiked levels. Therefore, the developed method meets the requirements for the determination of THC in edible vegetable oil.

Key words: edible vegetable oil, δ9-Tetrahydrocannabinol, ultra-high performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS), negative ion mode

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