响应面优化固相萃取法测定化妆品中大麻素类化合物

doi:10.3969/j.issn.2097-2806.2026.02.016

摘要/Abstract

摘要：

建立了固相萃取结合高效液相色谱串联质谱（HPLC-MS/MS）测定化妆品中8种大麻素类化合物的分析方法。样品经乙腈超声提取后过EMR-Lipid固相萃取小柱净化，采用Waters ACQUITY UPLC BEH C₁₈色谱柱分离，乙腈-10 mmol/L乙酸铵溶液（含0.1%甲酸）流动相体系梯度洗脱，电喷雾离子源多反应监测模式进行检测。利用单因素和响应面优化得到最佳提取条件：乙腈体积为10 mL，超声时间为20 min，氯化钠加入质量为1 g。在该条件下，于低、中、高三水平添加质量浓度下，测得8种物质的平均回收率为85.1%~98.5%，相对标准偏差小于8.5%。各物质线性关系良好，相关系数R²均大于0.99；检出限为0.5~2.5 ng/g，定量限为1~5 ng/g。该方法定量准确，适用于化妆品中大麻素类化合物的定量检测。

关键词: 高效液相色谱串联质谱, EMR-Lipid固相萃取柱, 大麻素类化合物, 响应面优化

Abstract:

A new method was established for the determination of 8 cannabinoids in cosmetics by solid phase extraction（SPE）using high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）. The cosmetic samples were extracted with acetonitrile and ultrasonic extraction, then sodium chloride was added. After being vortexed and centrifuged, the liquid supernatant was purified with EMR-Lipid SPE. This SPE column could selectively remove large molecular substances such as lipids from cosmetic matrices, which has excellent purification effects. Then 8 cannabinoids were separated on a Waters ACQUITY UPLC BEH C₁₈ column by gradient elution using acetonitrile and 10 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid as mobile phases. The data were collected by electrospray ionization source and multiple reaction monitoring mode. Optimization was conducted using a three-factor and three-level response surface method for the best conditions of determination. The optimum determination conditions are acetonitrile volume: 10 mL; ultrasonic time: 20 min; sodium chloride mass: 1 g. Under this combination of conditions, the average recoveries are between 85.1% and 98.5% at three spiked levels, and the relative deviations are less than 8.5%. There are good linear relationships for 8 cannabinoids. The linear relationships（R²）are above 0.99. The limits of detection（LOD）range from 0.5 to 2.5 ng/g, and the limits of quantification（LOQ）range from 1 to 5 ng/g. The method is accurate and suitable for the determination of 8 cannabinoids in cosmetics.

Key words: HPLC-MS/MS, EMR-Lipid SPE, cannabinoids, response surface methodology

中图分类号:

TQ658

王玉梅, 刘真, 刘其南, 姜星, 黄浩伦, 孙小杰. 响应面优化固相萃取法测定化妆品中大麻素类化合物[J]. 日用化学工业（中英文）, 2026, 56(2): 271-276.

Yumei Wang, Zhen Liu, Qinan Liu, Xing Jiang, Haolun Huang, Xiaojie Sun. Determination of cannabinoids in cosmetics by solid phase extraction with response surface methodology[J]. China Surfactant Detergent & Cosmetics, 2026, 56(2): 271-276.

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参考文献 19

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序号	化合物	保留时间/min	母离子(m/z)	子离子(m/z)	碰撞电压/V	裂解电压/V
1	CBDV	5.68	287	165^*，135	20，26	80
2	CBDA	5.95	357	339^*，245	-20，-30	-100
3	CBG	6.19	317	193^*，123	18，20	105
4	CBD	6.25	315	259^*，193	18，20	100
5	THCB	6.37	287	165^*，135	18，22	80
6	CBN	6.77	311	293^*，223	25，34	90
7	THCA-A	6.99	357	313^*，245	-16，-20	-80
8	THC	7.06	315	259^*，193	22，26	100

编号	编码水平			大麻二酚回收率/%
编号	A	B	C	大麻二酚回收率/%
1	0	0	0	91.1
2	1	0	0	92.8
3	-1	1	0	77.6
4	0	1	1	85.9
5	1	0	1	89.9
6	1	1	0	90.3
7	0	0	0	90.5
8	0	-1	1	80.5
9	-1	0	-1	79.5
10	0	0	0	93.5
11	0	0	0	91.2
12	1	-1	0	80.5
13	-1	-1	0	78.5
14	0	-1	-1	79.6
15	1	0	-1	83.6
16	-1	0	1	75.6
17	0	1	-1	82.7

方差来源	方差和	自由度 (d f)	均方	F值	P值	显著性
Model	575.74	9	63.97	52.56	<0.000 1	显著
A	136.95	1	136.95	112.51	<0.000 1	显著
B	37.85	1	37.85	31.09	0.000 8	显著
C	5.28	1	5.28	4.34	0.075 8
AB	28.62	1	28.62	23.51	0.001 9	显著
AC	26.01	1	26.01	21.37	0.002 4	显著
BC	1.32	1	1.32	1.09	0.331 9
A ²	107.80	1	107.80	88.57	<0.000 1	显著
B ²	106.74	1	106.74	87.69	<0.000 1	显著
C ²	89.48	1	89.48	73.51	<0.000 1	显著
Residual	8.52	7	1.22
Lack of fit	2.09	3	0.697 5	0.434 0	0.740 6	不显著
Pure error	6.43	4	1.61
Cor total	584.26	16
	CV=1.30%；AdjR²=0.966 7