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日用化学工业 ›› 2021, Vol. 51 ›› Issue (2): 166-170.doi: 10.3969/j.issn.1001-1803.2021.02.014

• 分析与检测 • 上一篇    

超高效液相色谱-串联质谱法测定化妆品中的大麻二酚

李硕(),李莉(),王海燕,孙磊   

  1. 中国食品药品检定研究院,北京 100050
  • 收稿日期:2020-05-21 修回日期:2021-01-19 出版日期:2021-02-22 发布日期:2021-02-22
  • 通讯作者: 李莉
  • 作者简介:李 硕(1986-),男,工程师,硕士,电话:(010)67095064,E-mail: pahayokolide@sina.com

Determination of cannabidiol in cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry

LI Shuo(),LI Li(),WANG Hai-yan,SUN Lei   

  1. National Institutes for Food and Drug Control, Beijing 100050, China
  • Received:2020-05-21 Revised:2021-01-19 Online:2021-02-22 Published:2021-02-22
  • Contact: Li LI

摘要:

建立了一种化妆品中大麻二酚(CBD)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析检测方法。样品用甲醇超声提取,采用超滤型净化柱净化,外标法定量。采用CAPCELL CORE ADME色谱柱(2.1 mm×100 mm,2.7 μm);流动相为含有0.1%甲酸的水溶液(A)-0.1%甲酸的乙腈溶液(B),进行梯度洗脱;质谱采用电喷雾离子源(ESI),在正离子多反应监测模式下进行检测。结果表明,CBD在0.5~100 μg/L质量浓度范围内线性关系良好,相关系数r=0.999 9;检出限(LOD)为1 μg/kg,定量限(LOQ)为3 μg/kg;2个添加质量浓度下回收率为76.6%~110.2%,RSD值(n=6)为1.4%~7.7%。本方法分析时间短、准确性好、灵敏度高,可用于化妆品中大麻二酚的定性及定量分析。

关键词: 大麻二酚, 化妆品, 超高效液相色谱-串联质谱法

Abstract:

An analytical method of ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for determination of cannabidiol (CBD) in cosmetics. The samples were extracted with methanol under ultrasonic condition and then purified with an ultrafiltration type purification column before quantitative analysis by external standard method. The UPLC separation was carried out on a CACELL CORE ADME column (2.1 mm×100 mm, 2.7 μm) by gradient elution using aqueous solution containing 0.1% formic acid (A)- acetonitrile solution containing 0.1% formic acid (B). The electrospray ionization source in positive ion mode (ESI) was used for both qualitative and quantitative analysis of CBD in the multiple reaction monitoring (MRM) mode. The results show that the established method exhibits a good linear relationship in the corresponding concentration range of 0.5-100 μg/L with a correlation coefficient r=0.999 9. The limit of detection (LOD) is 1 μg/kg and the limit of quantification (LOQ) is 3 μg/kg. The recoveries of standard addition at two different levels are 76.6%-110.2% while the relative standard deviation (n=6) are 1.4%-7.7%. Accurate and sensitive UPLC-MS/MS method was developed and validated. This method is suitable for qualitative and quantitative analysis of cannabidiol in cosmetics.

Key words: cannabidiol, cosmetics, ultra-performance liquid chromatography-tandem mass spectrometry

中图分类号: 

  • TQ658