HPLC测定儿童化妆品中10种邻苯二甲酸酯类化合物的含量

doi:10.3969/j.issn.1001-1803.2019.03.013

Abstract

Abstract:

A sensitive and rapid method was developed for the determination of 10 phthalate esters （PAEs） in children’s cosmetics by high performance liquid chromatography （HPLC）. The analytes were tested with an Acclaim ^TM 120-C₁₈ reversed-phase column （4.6 mm×250 mm, 5 μm） under the gradient elution of methanol, acetonitrile and water, and subsequently detected by Diode Array Detector （DAD） at 280 nm. The flow rate was set at 1.0 mL/min. The results show that the ten compounds show good linearity within the concentration range of 1-100 mg/L. The corresponding linear correlation coefficients are all equal to or greater than 0.999 6. And the limits of detection and quantification （LOD and LOQ） located at the range of 0.2-5.0 mg/L and 0.5- 10.0 mg/L, respectively. Recovery experiments were then carried out with 8 cosmetic samples （lotion, cream and oily cosmetics）. The average recoveries are between 89.2% and 106.1% with relative standard deviations <5%. Results show that it is a simple and accurate method with low LOD which can serve for cosmetics supervision in determination of the PAEs. One of the eight cosmetics was verified as a positive sample, and three methods were applied to confirm this result.

Key words: children’s cosmetics;, phthalate ester, high performance liquid chromatography

CLC Number:

TQ658

Yong-chao YANG,Jing YAN,Hao-li-bao ZHAO,Xue-yang LI,Yuan ZHANG,Lei ZHOU. Determination of 10 phthalate esters in cosmetics for children by HPLC[J].China Surfactant Detergent & Cosmetics, 2019, 49(3): 203-208.

Figures/Tables 8

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References 20

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化合物	线性回归方程	相关系数r
DMP	y = 0.030 6 x - 0.002 3	0.999 9
DEP	y = 0.026 3 x - 0.003 6	0.999 9
DPP	y = 0.022 7 x - 0.005 5	0.999 9
DBP	y = 0.019 3 x - 0.009 2	0.999 6
DAP	y = 0.020 7 x - 0.010 8	0.999 6
DHP	y = 0.017 2 x - 0.004 9	0.999 9
BBP	y = 0.016 6 x - 0.001 5	0.999 9
DCHP	y = 0.013 9 x - 0.002 3	0.999 9
DOP	y = 0.015 4 x + 0.000 6	0.999 9
DEHP	y = 0.014 3 x - 0.000 6	0.999 9

化合物	化妆品（水状）			化妆品（霜乳状）			化妆品（油状）
化合物	ρ/（mg·L^-1）	回收率/%	RSD/%	ρ/（mg·L^-1）	回收率/%	RSD/%	ρ/（mg·L^-1）	回收率/%	RSD/%
DMP	20.72	103.6	0.84	19.89	99.4	1.34	19.97	99.8	1.17
DEP	18.10	90.5	0.94	20.73	103.6	1.30	19.96	99.8	0.65
DPP	20.33	101.6	1.19	19.72	98.6	1.56	19.16	95.8	1.67
DBP	20.22	101.1	1.38	20.89	104.4	0.93	19.82	99.1	0.96
DAP	19.56	97.8	2.23	20.66	103.3	0.90	19.94	99.7	1.21
DHP	20.00	100.0	1.85	20.73	103.7	1.36	20.65	103.3	0.32
BBP	20.45	102.3	1.55	20.29	101.5	0.66	20.09	100.5	1.00
DCHP	21.22	106.1	1.56	20.74	103.7	0.75	20.21	101.1	1.24
DOP	19.43	97.2	1.43	19.98	99.9	3.27	19.49	97.5	1.62
DEHP	19.12	95.6	1.99	19.41	97.1	1.62	17.84	89.2	1.96

编号	含量/（μg·g^-1）
编号	DMP	DEP	DPP	DBP	DAP	DHP	BBP	DCHP	DOP	DEHP
1#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
2#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	6 573.6
3#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
4#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
5#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
6#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
7#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.
8#	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.	N.D.

Determination of 10 phthalate esters in cosmetics for children by HPLC

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化合物	检出限/（mg·L^-1）	定量限/（mg·L^-1）	检出浓度/（μg·g^-1）	最低定量浓度/（μg·g^-1）
DMP	0.2	0.5	2.0	5.0
DEP	0.3	0.5	3.0	5.0
DPP	0.4	1.0	4.0	10
DBP	5.0	10.0	50	100
DAP	5.0	10.0	50	100
DHP	2.0	6.0	20	60
BBP	2.0	8.0	20	80
DCHP	2.0	4.0	20	40
DOP	5.0	7.0	50	70
DEHP	1.0	4.0	10	40

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t/min	φ（甲醇）/%	φ（乙腈）/%	φ（水）/%
0	10	20	70
6	10	20	70
11	5	0	95
24	5	0	95
25	10	20	70