浊点萃取-高效液相色谱法检测化妆品中4种合成酚类抗氧化剂

doi:10.3969/j.issn.1001-1803.2020.07.012

Abstract

Abstract:

A high performance liquid chromatography （HPLC） method was developed for the simultaneous determination of 4 synthetic phenolic antioxidants （SPAs） in cosmetics, including propyl gallate, tertiary butyl hydroquinone, butylated hydroxyanisole, and butylated hydroxytoluene. The samples were extracted by ultrasound-assisted cloud point extraction （CPE） with PEG-12 dimethylsiloxane （DC-193） as the extraction solvent. Fatty acid was added to decrease the cloud point of DC-193. When the volume fraction of nonanoic acid was 10%, it was the best in terms of cloud point, phase separation speed and extraction rate. Then multi-response surface method was used to optimize CPE. The optimum conditions of CPE were: φ （DC-193） of 2.5%, ultrasound time of 30 min, equilibrium temperature at 67 ℃, and equilibrium time of 57 min. The external standard method was used for quantification. The results show that the linear correlation coefficients of the 4 SPAs were all greater than 0.99. The average recoveries at three spiked levels were in the range of 84%-91% with RSDs of 1.2%-2.3%.

Key words: cloud point extraction, high performance liquid chromatography, cosmetics, synthetic phenolic antioxidants

CLC Number:

TQ658

CHEN Miao,LI Li-xian,KONG Xiang-ye,GAO Ying,YANG Ya-ling. Determination of four synthetic phenolic antioxidants in cosmetics by cloud point extraction-high performance liquid chromatography[J].China Surfactant Detergent & Cosmetics, 2020, 50(7): 504-508.

Figures/Tables 8

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References 11

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	A 平衡温度/ C	B φ(DC-193)/%	C 平衡时间/min	D 超声时间/min
最大值	95	10	132.5	87.5
最小值	25	1	5	5
平均值	62	3.78	50	34

方差来源	平方和	自由度	均方	F值	Prob﹥F
模型	15 959.2	14	1 139.9	56.8	﹤0.000 1*
A	1 421.3	1	1 421.3	70.8	﹤0.000 1*
B	9.9	1	9.8	0.4	0.049 4*
C	290.4	1	290.4	14.5	0.001 7*
D	407.3	1	407.3	20.3	0.000 4*
AB	850.8	1	850.8	42.4	﹤0.000 1*
AC	3.8	1	3.8	0.2	0.667 8
AD	243.6	1	243.6	12.1	0.003 3*
BC	67.8	1	67.7	3.4	0.086 1*
BD	293.9	1	293.9	14.6	0.001 6*
CD	1.2	1	1.2	0.1	0.807 5
A²	2 334.9	1	2 334.9	116.4	﹤0.000 1*
B²	969.1	1	969.1	48.3	﹤0.000 1*
C²	16.0	1	16.0	0.8	0.385 9
D²	36.5	1	36.5	1.8	0.197 3
残差	300.9	15	20.1
总和	16 260.2	29

合成酚类抗氧化剂	线性方程	相关系数	线性范围/（mg·L^-1）	检出限/（mg·L^-1）
PG	y = 136.06x+21.43	0.999 9	1~500	0.20
TBHQ	y = 39.36x+6.40	0.999 9	1~500	1.10
BHA	y = 41.31x+8.39	0.999 8	1~500	0.40
BHT	y = 25.77x+3.68	0.999 9	1~500	0.85

合成酚类抗氧化剂	加标量/（mg·kg^-1）	回收量/（mg·kg^-1）（RSD/%）			回收率/%
合成酚类抗氧化剂	加标量/（mg·kg^-1）	第一天	第二天	第三天	回收率/%
PG	25	21 （2.1）	21 （2.0）	21 （1.8）	84
	50	45 （1.9）	43 （1.9）	42 （1.6）	87
	75	65 （1.2）	66 （1.4）	64 （1.7）	87
TBHQ	25	22 （2.0）	21 （2.0）	21 （1.8）	86
	50	43 （1.8）	44 （1.9）	43 （1.7）	86
	75	64 （1.7）	66 （1.5）	65 （1.8）	87
BHA	25	23 （2.0）	22 （1.9）	22 （2.3）	89
	50	45 （1.8）	44 （1.9）	45 （1.8）	89
	75	68 （1.5）	67 （1.3）	67 （1.2）	90
BHT	25	22 （1.9）	23 （2.1）	21 （1.8）	85
	50	45 （2.0）	45 （1.9）	43 （1.6）	89
	75	67 （1.7）	68 （1.5）	67 （1.6）	91

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Determination of four synthetic phenolic antioxidants in cosmetics by cloud point extraction-high performance liquid chromatography

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