Determination Of Phthalic Acid Esters In Cosmetics By Liquid Chromatography Tandem Mass Spectrometry

Phthalic acid esters is the most common plasticizer in plastic industry, which iswidely used in polymeric materials, such as polyvinyl chloride (PVC), polyvinylacetate (PVAC). Phthalic acid esters added to the plastic can enhance the transparency,elasticity and service life of plastic. Because of phthalic acid esters have goodlubricity and ductility, adding in liquid cosmetics, perfume, nail polish, shampoo,detergent and other can increase the smoothness, adding in nail polish can increase theadhesion.Plastic packaging is the most widely used in the field of cosmetics, in particular,ordinary middle and low cosmetics. The research finds that Phthalic acid esters caneasily migrate from the plastic to cosmetics, especially in high oil content and highsolvent content.Research reports of phthalic acid esters is a kind of environmental estrogen,excessive intake will cause a certain impact on animal reproduction and fertility, butalso increase the burden on the liver and kidney, the toxicity of phthalate acid esters ismainly reflected in reproduction and fertility. Along with the social development, thepeople living standard universal enhancement, the cosmetics already become one ofthe essential consumer goods. The quality of cosmetics is related to people’s health,the quality and safety of the problem has caused the attention of the governments ofthe world..In this paper, the main content is to construct liquid chromatography tandemmass spectrometry detection phthalic acid esters in cosmetics and plastic packagingmaterials. to raise the accuracy and reliability for the recovery rate test and precisionverification.18kinds of cosmetics and9kinds of cosmetic packaging samples weredetected by the method of this research..Objective:To establish the method for detecting phthalic acid esters in the cosmetic and inthe cosmetic plastic packaging with liquid chromatography tandem mass spectrometry. It has completed the detection of phthalic acid esters of18types of cosmetic as wellas of9packaging for cosmetic.Methods:In this paper, using Ultrasonic to extracted the Phthalic acid esters in thecosmetic samples as well as in cosmetic plastic packaging and investigating theinfluences of time and extraction solvent on the extraction rate for phthalic acid estersin the cosmetic.The extracts from cosmetic and the packaging samples would bepurified by using the Solid Phase Extraction method, investigating various SolidPhase Extraction columns, eluent and the influence of eluent volume on the purifyingeffect of the extracts from the cosmetic and the cosmetic packaging samples.The Phthalic acid esters from the samples would be analyzed by using the liquidchromatography tandem mass spectrometry method, to raise the accuracies for therecovery test along with the verification methods of precision degree.Results:Methanol was adopted as the extraction solvent, extraction time was15minutes,extraction frequencies were twice, The recoveries for21PAEs in liquid cosmeticswere all exceeded84.2%. Add6mL acetone6mL n-hexane for activation beforeadding the sample then5%acetone in n-hexane used for elution. The recoveries morethan89.6%. Methanol was adopted as the extraction solvent, extraction time was30minutes, extraction frequencies were twice, The recoveries for21phthalic acid estersin Cream, milk cosmetics as well as in cosmetic plastic packaging were all exceeded80.1%.Add6mL acetone6mL n-hexane for activation before adding the sample then5%acetone in n-hexane used for elution. The recoveries more than84.5%. Whenliquid chromatography tandem mass spectrometry was used as method of testing forphthalic acid esters from cosmetic and its plastic packaging, showed that the recoveryrate of phthalic acid esters was84.5%～115.4%, Relative Standard Deviation（RSD）was2.3%～12.5%, The calibration curves of21phthalic acid esters in1ng.mL-1~100ng.mL-1range obtained were linear with correlation coefficients greater than0.997. The detection limit (3S/N) of0.1~1ng.mL-1, the limit of quantification (10S/N) for0.4~3ng.mL-1.Conclusion:This research has established the method for detecting phthalic acid esters in thecosmetic and in the cosmetic plastic packaging with the liquid chromatography tandem mass spectrometry. It is confirming the extraction condition and purificationcondition of solid phase extraction for phthalic acid esters from the samples. Thedetection limit of the method for phthalic acid esters are0.1～1ng.mL-1, for cosmeticsand plastic packaging of its testing standard has the reference value. The methodestablished were applied to detect21phthalic acid esters in18cosmetic productsPaste, emulsion, aqueous cosmetics and9Plastic packaging of cosmetics on sale withsatisfactory results. Test results showed that there are11kinds of cosmetics containPhthalic acid esters,6kinds of cosmetic plastic packaging materials contain Phthalicacid esters.