QuEChERS-UPLC法测定化妆品中10种性激素

doi:10.3969/j.issn.1001-1803.2021.09.016

Abstract

Abstract:

A method of QuEChERS coupled with ultra-high performance liquid chromatography was developed for determination of 10 sex hormones in cosmetics. The sample was dispersed using saturated sodium chloride, and purified by QuEChERS after acetonitrile ultrasound extraction. Chromatographic separation was achieved on a CORTECS C₁₈+ column （2.1 mm×100 mm, 2.7 μm） by gradient elution using acetonitrile-water as mobile phase. PDA detector was used to test samples at multiple wavelengths, and external standard method was used for quantification. Results show that there is a good linear relationship for each of the 10 sex hormones in respective mass concentration range with their correlation coefficients （r） all above 0.99. The limits of detection （LOD） and the limits of quantitation（LOQ） for the 10 sex hormones are in the range of 0.02-0.1 μg/mL and 0.05-0.3 μg/mL, respectively. Average recoveries at three levels of 5, 25 and 50 μg/g are in the range of 81.2%-103.5%, with relative standard deviations （RSD, n=6） of 0.5%-12.0%. With the advantages of simplicity and good reproducibility, this method is suitable for the analysis of sex hormones in cosmetics.

Key words: QuEChERS, ultra-high performance liquid chromatography, cosmetics, sex hormone, determination

CLC Number:

TQ658

Hu Bei,Li Lixia,Liu Hong,Huang Wei,Ding Xiaoping. Determination of 10 sex hormones in cosmetics by QuEChERS-UPLC[J].China Surfactant Detergent & Cosmetics, 2021, 51(9): 918-924.

Figures/Tables 6

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Tab. 1

Tab. 2

References 21

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化合物	线性范围/ （μg·mL^-1）	相关系数r			检出限/（μg·mL^-1）	定量限/（μg·mL^-1）
化合物	线性范围/ （μg·mL^-1）	水状	乳状	霜状	检出限/（μg·mL^-1）	定量限/（μg·mL^-1）
肾上腺甾酮	0.5~20.7	0.999 5	0.999 4	0.999 9	0.03	0.1
群勃龙	0.5~18.5	0.999 8	0.999 7	0.999 9	0.03	0.1
诺龙	0.5~19.1	0.999 7	0.999 8	0.994 0	0.05	0.2
美雄酮	0.6~24.1	0.999 5	0.999 8	0.994 1	0.06	0.2
炔诺酮	0.5~21.7	0.999 1	0.999 7	0.994 0	0.05	0.2
21-羟基孕酮	0.5~19.5	0.999 7	0.999 8	0.993 6	0.1	0.3
雄烯二酮	0.5~20.6	0.999 1	0.999 8	0.994 8	0.1	0.3
孕二烯酮	0.5~20.0	0.998 7	0.999 6	0.993 7	0.1	0.3
氯司替勃	0.5~20.1	0.999 0	0.999 4	0.996 1	0.03	0.1
甲羟孕酮	0.5~19.5	0.998 8	0.999 5	0.995 5	0.02	0.05

化合物	加入量/（μg·g^-1）	水状		乳状		膏状
化合物	加入量/（μg·g^-1）	平均回收率/%	相对标准偏差RSD/%	平均回收率/%	相对标准偏差RSD/%	平均回收率/%	相对标准偏差RSD/%
肾上腺甾酮	5	92.4	4.0	84.9	6.3	85.5	6.7
	25	96.1	1.4	90.8	2.7	90.5	5.2
	50	98.5	0.6	96.9	2.7	95.1	4.5
群勃龙	5	93.4	0.8	82.3	7.5	95.0	4.3
	25	95.3	0.8	92.2	5.6	90.6	5.0
	50	98.6	1.6	98.6	2.1	95.2	4.4
诺龙	5	95.1	1.3	85.6	9.6	93.8	4.8
	25	95.2	0.7	92.7	6.3	90.0	4.8
	50	98.7	1.1	99.0	2.8	95.1	4.5
美雄酮	5	92.0	0.5	83.1	8.8	93.7	5.0
	25	95.0	0.7	92.8	6.4	89.3	4.2
	50	98.6	1.1	99.2	3.0	94.8	4.3
炔诺酮	5	89.2	1.1	84.3	9.4	95.2	5.3
	25	95.6	0.7	93.2	7.4	89.2	4.0
	50	98.6	1.1	99.8	3.7	94.6	4.3
21-羟基孕酮	5	92.1	0.7	82.5	8.9	92.9	7.5
	25	95.0	0.6	92.8	6.7	90.3	4.4
	50	98.7	1.1	99.2	3.1	95.0	4.5
雄烯二酮	5	92.0	1.0	83.9	11.3	95.0	5.1
	25	95.1	0.7	93.4	6.9	91.0	4.2
	50	98.6	1.2	99.8	3.3	94.6	4.5
孕二烯酮	5	90.2	1.5	85.2	12.0	98.4	5.4
	25	94.9	0.6	94.9	8.3	88.8	3.8
	50	98.6	1.0	101.2	4.7	94.0	4.4
氯司替勃	5	91.8	1.8	89.1	10.1	81.2	4.6
	25	94.6	1.0	96.5	8.9	89.2	4.5
	50	98.8	1.1	102.6	6.6	93.6	4.4
甲羟孕酮	5	92.5	1.2	88.3	11.9	86.3	8.1
	25	94.4	1.0	96.1	8.7	101.1	5.3
	50	98.5	1.1	103.5	6.3	97.6	8.7

Determination of 10 sex hormones in cosmetics by QuEChERS-UPLC

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