高效液相色谱-串联质谱法测定婴幼儿化妆品中微量丙烯酰胺

doi:10.3969/j.issn.1001-1803.2022.01.014

Abstract

Abstract:

To establish a liquid-liquid extraction HPLC-MS/MS method for the identification and quantification of acrylamide in three cosmetics matrixes. The cosmetics were dissolved in dichloromethane and the acrylamide was extracted with 0.1% formic acid. The extracted solution was separated on an ACE EXCEL 3 C18-AR （100×4.6 mm, 3 μm） chromatographic column with a mixture of 0.1% formic acid and acetonitrile as mobile phase for isocratic elution and detected with a triple quadrupole mass analyzer using ESI with positive ionization. Ions was monitored in the multiple reaction mode. The acrylamide was identified with relative retention time and ion abundance ratio, and quantified by internal standard method. The established method showed a good linearity in the mass concentration range of 2.5-2 500 μg/L with a LOQ of 0.025 mg/kg for acrylamide in three kinds of cosmetics matrix. The LOD of oil and emulsion matrix were 0.005 mg/kg, and the LOD of cream-like matrix was 0.008 mg/kg. The extraction recovery and precision were 86.9%-113.5% and 0.6%-10.4%, respectively. The established liquid-liquid extraction HPLC-MS/MS method is proved to be accurate and sensitive, and can be applied to determine acrylamide in different cosmetic products.

Key words: liquid-liquid extraction method, HPLC-MS/MS, acrylamide

CLC Number:

TQ658

Shao Fangxian,Li Geng,Chen Minhui. Determination of acrylamide residue in baby cosmetics by HPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2022, 52(1): 91-97.

Figures/Tables 6

Fig. 1

Tab. 1

Tab. 2

Tab. 3

Tab. 4

Tab. 5

References 15

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基质类型	方法号	方法一		方法二		方法三
基质类型	化合物	丙烯酰胺	内标	丙烯酰胺	内标	丙烯酰胺	内标
油状	基质效应/% ^*	100.8	100.4	93.0	93.4	95.4	90.8
	RSD/%	3.2	1.1	11.3	14.7	2.5	2.0
	内标校正的基质效应/% ^**	100.3		100.0		105.0
	RSD/%	3.9		3.8		2.3
乳状	基质效应/% ^*	27.8	28.9	56.4	57.7	77.7	80.6
	RSD/%	5.7	3.2	9.0	6.3	6.1	4.9
	内标校正的基质效应/% ^**	96.0		97.7		96.7
	RSD/%	2.5		2.9		2.5
膏霜类	基质效应/% ^*	48.8	55.2	119.9	125.9	72.0	77.5
	RSD/%	14.7	3.4	15.4	14.0	5.6	7.0
	内标校正的基质效应/% ^**	88.2		95.1		92.1
	RSD/%	12.7		1.5		2.7

基质类型	方法号	方法一		方法二		方法三
基质类型	化合物	丙烯酰胺	内标	丙烯酰胺	内标	丙烯酰胺	内标
油状	绝对提取回收率/%^*	103.6	99.3	79.6	81.2	90.8	93.9
	RSD/%	0.7	1.5	4.5	5.1	2.5	2.0
	提取回收率/%^**	104.3		97.5		96.7
	RSD/%	1.5		1.2		5.3
乳状	绝对提取回收率/%^*	102.0	95.3	82.0	82.3	80.0	85.6
	RSD/%	9.8	11.2	0.3	1.8	5.4	6.2
	提取回收率/%^**	107.1		99.6		93.4
	RSD/%	2.2		2.1		4.1
膏霜类	绝对提取回收率/%^*	91.3	85.9	50.0	54.3	82.4	92.2
	RSD/%	8.8	8.7	7.3	13.7	5.8	0.2
	提取回收率/%^**	106.5		92.6		88.4
	RSD/%	6.9		6.0		2.4

化合物	油状				乳状				膏霜类
化合物	基质效应/ %	RSD/ %	内标校正基质效应/%	RSD/ %	基质效应/ %	RSD/ %	内标校正基质效应/%	RSD/ %	基质效应/ %	RSD/ %	内标校正基质效应/%	RSD/ %
丙烯酰胺	90.3	8.2	99.8	5.4	85.4	10.8	99.7	6.6	79.0	9.7	97.8	6.9
内标	90.5	6.9			85.6	8.2			80.5	4.1

基质类型	标准曲线	相关系数r	检出限/（mg/kg）	定量限/（mg/kg）
油状	Y=0.409 7 X+0.016 06	r=0.999 8	0.005（SN=13）	0.025（SN=53）
乳状	Y=0.393 6 X-0.024 57	r=0.999 7	0.005（SN=7）	0.025（SN=18）
膏霜类	Y=0.351 2 X+0.020 97	r=0.999 5	0.008（SN=3）	0.025（SN=10）

基质类型	加入质量浓度/（µg/L）	测得质量浓度/（µg/L）	提取回收率/%	平均提取回收率/%	精密度/%
油状基质	4.954	4.969	100.3	101.3	1.7
		5.117	103.3
		4.969	100.3
	24.77	24.10	97.3	98.5	1.7
		24.23	97.8
		24.87	100.4
	123.8	126.0	101.8	99.0	2.6
		119.7	96.7
		122.1	98.6
乳状基质	4.954	4.473	90.3	88.3	2.0
		4.325	87.3
		4.325	87.3
	24.77	26.49	107.0	108.2	4.4
		28.11	113.5
		25.81	104.2
	123.8	137.8	111.3	110.6	0.6
		136.1	109.9
		137.0	110.7
膏霜类基质	4.954	4.647	93.8	89.6	4.1
		4.369	88.2
		4.305	86.9
	24.77	25.75	103.9	98.7	4.6
		23.91	96.54
		23.69	95.62
	123.8	116.7	94.3	97.4	10.4
		110.3	89.1
		134.6	108.7

Determination of acrylamide residue in baby cosmetics by HPLC-MS/MS

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