Liquid Chromatography And Mass Spectrometry Using To Screen And Detect Pharmaceutcals And Personal Care Produtcs In Environment And Food

With the development of the scientific technology and people's consumption level,Pharmaceutical and personal care products(PPCPs),as the necessity of human life,are ever-growing in the application ranges and the usage amounts.But that's the reason that give rise to the long-term existence of PPCPs in the environment characterized by the low concentration and large number with the wastes being discharged.The toxicity of the PPCPs is mainly focused on the chronic toxicity by long-term accumulated,which will not reveal until accumulated to a certain degree,potentially threatening the human health and environmental safety.Therefore,it's very necessary to have a effective testing on the PPCPs.This thesis mainly studies on the some of PPCPs testing methods in the fields of environment and food.In the aspect of planting environment,we screen and confirm the high content contaminants of the reclaimed water for the use of irrigation and test the polycyclic aromatic hydrocarbons(PAHs)easily accumulated in the planting soil.In the aspect of the animal-derived food safety,we optimize the testing methods of cephalosporins in milk.The main contents of our work are as follows:1.In this thesis,we have a screening and confirmation on the main PPCPs contaminants existing in the reclaimed water of the two agricultural irrigation rivers in Beijing.We use the method of the SPE to enrich the reclaimed water samples and then we screen the contaminants of the samples by the means of the UPLC-Q-TOF.We make comparisons between database and relative references,and verify by the means of UPLC-MS/MS to finally confirm the 16 kinds of high content PPCPs in total,including azithromycin,climbazole,ofloxacin,metoprolol,mexacarbate,propafenone,roxithromycin,telmisartan,levocetirizine,irbesartan,atrazine,prometryn,dimethomorph,rhodamine B,gliclazide,and tris(2-butoxyethyl)phosphate(TBEP).Using UPLC-MS/MS to make a quantitative evaluation to the PPCPs and the LOD is from 0.2ng/L to 8ng/L,the LOQ is from 0.3ng/L to 10ng/L,the linear correlation coefficient(R2)is greater than 0.99,the RSD is less than 15%.And the maximum content range of the PPCPs contaminants is from 6ng/L to 4.9?g/L existing in the reclaimed water samples.2.In the terms of investigation to the soil around the rivers,we should give priority to testing of PAHs,which is a kind of persistent organic pollutants(POPs).In this thesis,by the approach of MAE,we totally extract the 16 kinds of PAHs in the soil,including naphthalene(Nap),acenaphthene(Ace),acenaphthylene(Acy),fluorene(Fle),anthracene(Ant),phenanthrene(Phe),fluoranthene(Fla),pyrene(Pyr),benzo[a]anthracene(BaA),chrysene(Chy),benzo[b]fluoranthene(BbF),benzo[k]fluoranthene(BkF),benzo[a]pyrene(BaP),indeno[1,2,3-cd]pyrene(InP),dibenzo[a,h]anthracene(DBahA),benzo[g,h,i]perylene(BghiP).And then we optimize the extraction condition of those PAHs by RSM.From the study,100? as the extraction temperature,16 minutes as the extraction time,15mL as the dosage of extraction solvent,are all the best extracting conditions.Using UPCC to have a quantitative detection on those PAHs.According to the test,the LOD is from 2.5?g/Kg to 7.5?g/Kg,the LOQ is from 5?g/Kg to 15?g/Kg,the linear correlation coefficient(R2)is greater than 0.99,and the RSD is less than 18.9%.With regard to the PAHs existing in the soil samples,we only test that BaP has higher adsorption in the soil particles,and the content of the BaP can reach 596?g/Kg in soil.3.Milk is a kind of animal-derived food.In this thesis,we also use the methods of SPE to extract and purify the AmpC in milk,which is one of the antibiotics.We have established and optimized the testing methods with Weak-anion-exchange(WAX)SPE Column,and meanwhile,we enrich and test the 7 kinds of substances as follows,cefminox,cefotaxime,cefoperazone,cefixime,cefetametpivoxyl,cefalotin,cefuroxime.By the means of the quantitative analysis,we use the UPLC-MS/MS to test the LOD is from 0.05ng/mL to 2.4 ng/mL,the LOQ is from 0.1 ng/mL to 3.2 ng/mL,the recovery rate is between 47.63%and 114.62%,the linear correlation coefficient(R2)is greater than 0.99,and the RSD is less than 13.66%.According to the tests of milk selling in the urban,we have not find any above AmpC in it.