食品科学 ›› 2022, Vol. 43 ›› Issue (24): 357-364.doi: 10.7506/spkx1002-6630-20220331-385

• 安全检测 • 上一篇    

固相萃取-气相色谱质谱法测定食品中9 种大麻素

唐庆强,夏林兵,曹丹,杨方,吴春灯,薛昆鹏   

  1. (1.福州海关技术中心,福建 福州 350001;2.三明海关综合技术服务中心,福建 三明 365001;3.杭州国际旅行卫生保健中心(杭州海关口岸门诊部),浙江 杭州 310016;4.金华海关综合技术服务中心,浙江 金华 321001;5.浙江月旭材料科技有限公司,浙江 金华 321001)
  • 发布日期:2022-12-28
  • 基金资助:
    福建省自然科学基金项目(2020J1098);福建省科技计划项目(2021I0033); 海关总署科研项目(2020HK188;2021HK197);福州市科技计划项目(2020-S-34)

Determination of Nine Cannabinoids in Foods by Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

TANG Qingqiang, XIA Linbing, CAO Dan, YANG Fang, WU Chundeng, XUE Kunpeng   

  1. (1. Fuzhou Customs Technical Centre, Fuzhou 350001, China; 2. Sanming Customs Comprehensive Technology Service Center, Sanming 365001, China; 3. Hangzhou International Travel Healthcare Center (Hangzhou Customs Port Clinic), Hangzhou 310016, China; 4. Jinhua Customs Comprehensive Technology Service Center, Jinhua 321001, China; 5. Welch Materials (Zhejiang) Co. Ltd., Jinhua 321001, China)
  • Published:2022-12-28

摘要: 建立了测定橄榄油、猪肉、面包等食品中包括合成大麻在内9 种大麻素的气相色谱-质谱分析方法。样品经甲醇和乙腈提取、固相萃取净化以及HP-5MS毛细管色谱柱分离,使用电子电离源、选择离子监测模式以及外标法定量。结果表明:该方法在10~500 μg/L质量浓度范围内有良好线性关系,相关系数均大于0.999 2;方法的检出限(信噪比为3)和定量限(信噪比为10)分别为1~15 μg/kg和2.5~50 μg/kg。对不同样品基质进行1、2、10 倍定量限3 个水平的加标回收实验,9 种大麻素化合物的回收率为65.2%~117.9%,相对标准偏差为2.0%~12.7%。该方法灵敏度高、检测速度快、适用性强,对发现和控制我国食品中大麻素类物质的残留、制定检测标准和采取相应的管理措施具有一定的理论和现实意义。

关键词: 大麻素;合成大麻;气相色谱-质谱技术

Abstract: In this study, an analytical method based on gas chromatography-mass spectrometry (GC-MS) was developed for the determination of nine cannabinoid compounds in foods such as olive oil, pork and bread. The samples were extracted with methanol or acetonitrile, and the extract was purified on a solid phase extraction column. The target compounds were separated on an Agilent HP-5MS column. The instrument was operated using an electrospray ionization source (EIS) in the selected ion monitoring (SIM) mode. The external standard method was used for quantification. This method showed good linearity in the concentration range of 10–500 μg/L with correlation coefficients greater than 0.999 2. The limits of detection (LOD, RSN = 3) and limits of quantification (LOQ, RSN = 10) of the developed method were 1–15 and 2.5–50 μg/kg. The average recoveries of the nine cannabinoids from negative samples of different matrices spiked at LOQ, 2 × LOQ and 10 × LOQ concentrations ranged from 65.2% to 117.9%, with relative standard deviations (RSDs) between 2.0% and 12.7%. This method is very sensitive, fast, highly applicable, and useful for the detection of cannabinoid residues in foods.

Key words: cannabinoids; synthetic cannabinoids; gas chromatography-mass spectrometry

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