HPLC测定儿童化妆品中10种邻苯二甲酸酯类化合物的含量
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摘要
建立了测定儿童化妆品中10种邻苯二甲酸酯类(PAEs)化合物含量的高效液相色谱(HPLC)法。采用AcclaimTM 120-C18(4.6 mm×250 mm, 5 μm)反相柱,流动相为甲醇-乙腈-水,梯度洗脱,流速1.0 mL/min,二极管阵列检测器(DAD),检测波长280 nm。结果表明,在1～100 mg/L范围内,10种PAEs的质量浓度与峰面积呈现良好的线性关系,相关系数均≥0.999 6,10种PAEs的检出限和定量限分别在0.2～5.0 mg/L和0.5～10.0 mg/L范围内。方法验证过程中做了3类化妆品共计8种(化妆水、霜乳类和油状)样品的添加回收,平均回收率为89.2%～106.1%,RSD均小于5%。该方法简便准确,检测限较低,满足实际检测需要,可用于化妆品中PAEs的检测。1个样品有检出,通过3种方法确证为阳性。
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 AcclaimTM 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.
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 AcclaimTM 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.
引文
[1]Wang Xin.Studies on the determination and migration of phthalate esters in food[D].Wuxi:Jiangnan University,2008.
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[13]Bai Yamin,Yang Xiaoshan,Mao Qing,et al.Determination of ten kinds of phthalic acid ester in cosmetics by LC-MS[J].China Surfactant Detergent&Cosmetics,2014,44(8):472-475.
[14]Hu Lei,Li Yinghong,Liu Chenchen,et al.Determination of 16 kinds of phthalates in cosmetics by GC/QQQ-MS[J].Flavour Fragrance Cosmetics,2013,4:42-48.
[15]Llompart M,Celeiro M,Lamas J P,et al.Analysis of plasticizers and synthetic musks in cosmetic and personal care products by matrix solid-phase dispersion gas chromatography-mass spectrometry[J].Journal of Chromatography A,2013,1293:10-19.
[16]Cai Xia,Huang Yanting,Fu Meiyan,et al.Determination of 12 kinds of phthalates in cosmetics by HPLC[J].China Surfactant Detergent&Cosmetics,2018,48(7):415-418.
[17]Liu Xiangping,Huang Wei,Li Chunye,et al.Determination of dibutyl phthalate and bis(2-ethylhexyl)phthalate in cosmetics by gas chromatography-mass spectrometry[J].Journal of Environment and Health,2007,24(11):915-916.
[18]Yang Qinghua,Shi Yilan,Shi Yukun,et al.Determination and analysis of 17 phthalic acid esters content in drinking water of Nantong in2013[J].Chinese Journal of Health Laboratory Technology,2015,25(1):95-104.
[19]Xu Yong,Yu Jian,Han Jing,et al.Determination of phthalate acid esters in cosmetic by GC-MS[J].Chinese Journal of Health Laboratory Technology,2014,24(22):3211-3216.
[20]Liu Jun,Zou Qin,Ku Erbanjiang,et al.Determination of phthalates and adipates in Xinjiang characteristic cosmetics by gas chromatography[J].Chinese Journal of Health Laboratory Technology,2013,23(4):816-818.
[2]Inoue K,Kawaguchi M,Okada F,et al.Column-switching highperformance liquid chromatography electrospray mass spectrometry coupled with online of extraction for the determination of mono-and di-(2-ethylhexyl)phthalate in blood samples[J].Analytical and Bioanalytical Chemistry,2003,375:527-533.
[3]Huang Yonghui.Simultaneous determination of 22 phthalate ester plasticizers in plastics toys by gas chromatography-mass spectrometry[J].Plastics Science and Technology,2011,39(1):94-98.
[4]Tienpont B,David F,Dewulf E,et a1.Pitfalls and solutions for the trace determination of phthalates in water samples[J].Chromatographia,2005,61:365-370.
[5]Wei Danqi.Research progress on the analytical methods of phthalate esters in cosmetics[J].Strait Pharmaceutical Journal,2013,25(11):8-11.
[6]Yang Yanwei,Zhu Ying.Determination of 10 kinds of phthalates in cosmetics by high performance liquid chromatography[J].Journal of Environment and Health,2006,23(4):360-362.
[7]Bola?os P P,Frenich A G,Vidal J L M.Application of gas chromatography-triple quadrupole mass spectrometry in the quantification confirmation of pesticides and poly-chlorinated biphenyls in eggs at trace levels[J].Journal of Chromatography A,2007,1167(1):9-17.
[8]Li Liang,Si Jiliang.Introduction of environmental endocrine disruptors[J].Journal of Environment and Health,2002,18(2):241-242.
[9]Zhang Junhua,Zhao Yu’e,Zhou Yanli,et al.Investigation reports of safety use of cosmetics[J].Journal of Pharmaceutical Research,2014,33(11):676-678.
[10]Benson R.Hazard to the developing male reproductive system from cumulative exposure to phthalate esters-dibutyl phthalate,diisobutyl phthalate,butylbenzyl phthalate,diethylhexyl phthalate,dipentyl phthalate,and diisononyl phthalate[J].Regulatory Toxicology and Pharmacology,2009,53(2):90-101.
[11]Zheng Xianghua,Lin Liyi,Fang Enhua,et al.Determination of23 phthalate esters in food by solid-phase extraction coupled with gas chromatography-mass spectrometry[J].Chinese Journal of Chromatography,2012,30(1):27-32.
[12]China Food and Drug Administration.Safety and Technical Standards for Cosmetics 2015[S].Beijing:Standards Press of China,2016.
[13]Bai Yamin,Yang Xiaoshan,Mao Qing,et al.Determination of ten kinds of phthalic acid ester in cosmetics by LC-MS[J].China Surfactant Detergent&Cosmetics,2014,44(8):472-475.
[14]Hu Lei,Li Yinghong,Liu Chenchen,et al.Determination of 16 kinds of phthalates in cosmetics by GC/QQQ-MS[J].Flavour Fragrance Cosmetics,2013,4:42-48.
[15]Llompart M,Celeiro M,Lamas J P,et al.Analysis of plasticizers and synthetic musks in cosmetic and personal care products by matrix solid-phase dispersion gas chromatography-mass spectrometry[J].Journal of Chromatography A,2013,1293:10-19.
[16]Cai Xia,Huang Yanting,Fu Meiyan,et al.Determination of 12 kinds of phthalates in cosmetics by HPLC[J].China Surfactant Detergent&Cosmetics,2018,48(7):415-418.
[17]Liu Xiangping,Huang Wei,Li Chunye,et al.Determination of dibutyl phthalate and bis(2-ethylhexyl)phthalate in cosmetics by gas chromatography-mass spectrometry[J].Journal of Environment and Health,2007,24(11):915-916.
[18]Yang Qinghua,Shi Yilan,Shi Yukun,et al.Determination and analysis of 17 phthalic acid esters content in drinking water of Nantong in2013[J].Chinese Journal of Health Laboratory Technology,2015,25(1):95-104.
[19]Xu Yong,Yu Jian,Han Jing,et al.Determination of phthalate acid esters in cosmetic by GC-MS[J].Chinese Journal of Health Laboratory Technology,2014,24(22):3211-3216.
[20]Liu Jun,Zou Qin,Ku Erbanjiang,et al.Determination of phthalates and adipates in Xinjiang characteristic cosmetics by gas chromatography[J].Chinese Journal of Health Laboratory Technology,2013,23(4):816-818.