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Determination Of Nipagin Esters And Organophosphorus Flame Retardants By High Performance Liquid Chromatography-Tandem Mass Spectrometry

Posted on:2015-03-30Degree:MasterType:Thesis
Country:ChinaCandidate:X Y ZhangFull Text:PDF
GTID:2251330428490923Subject:Biomedical engineering
Abstract/Summary:PDF Full Text Request
With the improvement of living standard, more and more people are focusing on thequality of life, from the diet to spiritual life of all aspects. As the exposure of food andcosmetic safety events, a large number of people concern about the threat to health.Although the promulgated and implemented laws and regulations have been carried outstrict requirement on food, cosmetics and package materials, and some harmful substanceshave a sophisticated detection technology, more effective means of detection is necessary.High performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS)with its unique advantages, such as less interference matrix, special sensitivity andspecificity lead to broad application prospects. This paper discussed the application ofHPLC-MS/MS in analysis of food and cosmetics, focused on the detection of four nipaginesters in cookies and organic phosphates flame retardants (OPFRs) in cosmetic withplastic package.A feasible method has been developed for the determination of four nipagin esterssimultaneously in cookies by HPLC-MS/MS. The parameters have been investigated andoptimized which impact the experiments. Samples were extracted by ultrasonic withmethanol. The extract was concentrated and purified by oasis HLB solid-phase extraction(SPE) column. And then performed on a Agilent Extend-C18(15cm2.1μm,3.5μm)column by gradient elution with water(A) and methanol(B) as mobile phases. The multiplereaction monitoring (MRM) in negative mode with electro-spray ionization (ESI), andexternal standard was used for quantitative determination. This method has a good linearrelationship in the range of0.1~10ng/mL. The recoveries of4nipagin esters at threespiked concentration levels ranged from81.90%to92.41%with the relative standarddeviations (RSD) of6.55%~9.78%. The results indicated that the method is simple,good sensitivity and repeatability. This method provided the certain basis for the detectionof nipagin esters in more food, pharmaceuticals and cosmetics.A method for the detection of OPFRs in cosmetics with plastic package byHPLC-MS/MS was developed. The samples were extracted by methanol usingmicrowave-assisted extraction, purified by alumina-N solid phase extraction column(SPE). The analytes were separated by Kromasil Eternity-5-C18(15cm2.1μm,3.5μm) and detected using LC-MS/MS in positive ion mode with the mobile phases of water (A,containing0.02mol/L ammonium acetate) and methanol (B). The linearity of method wasgood in the range of the given concentration. The mean recoveries at the three spikedlevels were (82.9±6.33)%~(98.6±3.97)%with the RSD of3.42%~9.60%. Thismethod was suitable for detection of cosmetic with plastic package, which had simpleoperation, low toxicity of reagents and good repeatability.Whether the OPFRs were added directly or in plastic package materials is not certain,so the detection of cosmetic plastic packaging materials is necessary. The samples wereextracted by ultrasonic with methanol, analyzed by optimized condition. The meanrecoveries at the three spiked levels were (81.8±3.11)%~(102.5±4.13)%with RSDof1.46%~5.02%. The results indicated that OPFRs neither existed in cosmetic nor plasticpackage. However, the detection method of migration is not perfect. We should makecosmetics simulation, so that we can simulated the real contact with the packagingmaterial in the process of migration characteristics, and also measuring the content oftarget substances which migrated from the molding materials or cosmetics simulation.This study laid a solid theoretical foundation for the detection of food and cosmetics.The HPLC-MS/MS has high practical value and broad application prospect.
Keywords/Search Tags:High performance liquid chromatography–tandem mass spectrometry(HPLC-MS/MS), Nipagin esters, organophosphorus flame retardants(OPFRs)
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