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Determination Of Some Contaminants In Condiments,Wine By Liquid Chromatography Tandem Mass Spectrometry

Posted on:2015-11-16Degree:MasterType:Thesis
Country:ChinaCandidate:J F QinFull Text:PDF
GTID:2321330488499097Subject:Analytical Chemistry
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Biogenic amine is a kind of alkaloid produced by decarboxylation of amino acid,which is essential to the body's metabolism.However,excess biogenic amine is harmful to nervous system.Bisphenol A is carcinogen,which is often found in plastic products.Because bisphenol A also can cause children sexual precocity,many countries prohibit its exist in children's products and food.Because of good antibacterial property,p-hydroxybenzoic acid esters are extensively applied in cosmetics,drugs and food.If p-hydroxybenzoic acid esters are intaked for long,they can make hazards to endocrine disorders.Beacause of accuracy,high selectivity and sensitivity,liquid chromatography tandem mass spectrometry(LC-MS/MS)method has been widely applied in food safety.This paper reviews the physical and chemical properties,hazards,toxicity mechanisms,content limit standards and common detection methods of common biogenic amines,p-hydroxybenzoic acid esters and bisphenol A(BPA).Through ultrasonic assisted extraction,LC-MS/MS methods are developed to determine biogenic amines and BPA in condiments,p-hydroxybenzoic acid esters in wine.The results are as follows:1.Through optimization of pretreatment method,1.0 mol·L-1 HCl was chosen as acidulant,the mixture of n-butanol and chloroform(4:6,v:v)were used as extraction agent.Using ultrasonic-assisted extraction,8 kinds of biogenic amines in condiments were simultaneously determined by LC-MS/MS with ESI+ ion source under multiple reaction monitoring(MRM)mode?Under gradient elution,8 kinds of biogenic amines can be completely separated within 15 minutes.Good correlation coefficients(r?0.9990)of 8 kinds of biogenic amines were obtained within their respective linear ranges.And the limit of detection(LOD)and limit of quantification(LOQ)ranged from 0.01 to 0.08 mg·kg-1 and 0.04 to 0.27 mg·kg-1,respectively.The mean recoveries of 8 kinds of biogenic amines ranged from 61.94%to 113.69%under 4 different spiked levels,and relative standard devitation(RSD)were 0.5%?7.4%.2.Using ethyl acetate as extraction agent under ultrasonic-assisted extraction,bisphenol A was determined in plastic packaged condiments by LC-MS/MS with ESI-ion source and MRM mode.In this method,the good linear ranges of bisphenol A was obtained with high correlation coefficient(r=0.9996).In vinegar and soy sauce,the LOD were 0.08 ?g·kg-1 and 0.12 ?g·kg-1,and LOQ were 0.27 ?g·kg-1 and 0.40 ?g·kg-1 respectively.Under 3 different spiked levels,the recoveries of bisphenol A ranged from 73.84%to 89.93%,and RSD were 6.3%?8.7%.3.Through ultrasound-assisted extraction with ethyl acetate as extraction agent,6 kinds of p-hydroxybenzoic acid esters in wine were simultaneously determined by LC-MS/MS with ESI-ion source under MRM mode.In this method,6 kinds of p-hydroxybenzoic acid esters can be completely separated within 18 minutes.Good correlation coefficients(r?0.9995)of 6 kinds of p-hydroxybenzoic acid esters were obtained within their respective linear ranges.And LOD and LOQ were in the range of 0.88?1.09 ?g·kg-1 and 2.95?3.62 ?g·kg-1,respectively.Under 3 different spiked levels,the average recoveries of 6 kinds of p-hydroxybenzoic acid esters were 65.09%?108.47%,and the RSD were 1.1%?12.1%.
Keywords/Search Tags:LC-MS/MS, condiments, wine, biogenic amine, bisphenol A p-hydroxybenzoic acid ester, determination
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