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Liang J.,Xiamen University | Liang J.,Fareast Testing and Technology Services Co. | Zhuang W.,Xiamen University | Wei D.,U.S. Food and Drug Administration | And 2 more authors.
Chinese Journal of Chromatography (Se Pu) | Year: 2012

A method was developed for the simultaneous determination of 19 phthalate esters (PAEs) at trace level in cosmetics by solid phase extraction (SPE) purification and gas chromatography-mass spectrometry (GC-MS) detection. The PAEs were extracted from cosmetic samples by dichloromethane with ultrasonic-assisted technique, purified by an SPE column packed with silica gel and neutral alumina (2:3, m/m) with the elution of 20 mL of mixed solvent of ethyl acetate-hexane (8:2, v/v). Qualitative and quantitative analysis were carried out by GC-MS in full scan and selected ion monitoring modes. The retention time of quantitative ions and the abundance ratio of characteristic ions were applied to rapidly and accurately identify each analyte so as to prevent the occurring of possible mistakes from complex matrix intervention. Under optimized conditions, the average recoveries for a shampoo sample spiked with the standards at 0.1, 0.5, 2.0 μg/g were in the range of 72.2% and 110.9%, and the relative standard deviations (RSDs) for the 19 PAEs were less than 10.3%(n=6) at the spiked level of 0.1 μg/g. The limits of detection (LODs, as 3 times of standard deviation) were between 0.0065 μg/g (for diisopentyl phthalate) and 0.062 μg/g (for diisobutyl phthalate). The method was successfully applied to the determination of the PAEs in 6 types of cosmetics. It is expected to promote the determination of the PAEs in other cosmetics with different matrices. © 2010 Editorial Office of Chinese Journal of Chromatography, Dalian Institute of Chemical Physics, CAS.

Wen Y.,Xiamen University | Wen Y.,Fareast Testing and Technology Services Co. | Ou Y.,Fareast Testing and Technology Services Co. | He M.,Fareast Testing and Technology Services Co. | Gong Z.,Xiamen University
Chinese Journal of Chromatography (Se Pu) | Year: 2013

A rapid determination method was developed for the quantification and confirmation of 22 carcinogenic aromatic amines derived from azo colorants in textiles and leather by ultra high performance liquid chromatography-tandem electrospray ionization mass spectrometry (UHPLC-MS/MS). The methods of EN 14362-1:2012 (for textiles) and ISO 17234-1:2010 (for leather) were adopted for sample pretreatment, finally diluted with methanol. The target compounds were separated by an Eclipse XDB-C18 RRHD column and eluted with methanol and water in gradient, and then determined by positive electrospray ionization mass spectrometry under multiple reaction monitoring (MRM) mode. The external standard method was used for the quantitative analysis. The separation conditions, fragment voltages, collision energies, etc. were optimized. The limits of quantification (LOQ) were below 0. 2 mg/kg for different compounds, matrix spike recoveries ranged from 70% to 120% at the spiked levels of 500, 1 000 and 1 500 μg/L, and the relative standard deviations (RSDs) were less than 15%. The proposed method is rapid, sensitive, accurate and selective.

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