The Research Of Major Exogenous Hazardous Substances Analysis In Areca Catechu Linn

Areca-nut is known as the seed of Areca catechu-----one of palmae plants.It is one of the four southern medicine in China(Areca catechu,Alpinia oxyphylla,Amomum villosum and Morinda offcinalis How.)and has the functions of sterilization,desinsectization,etc.Areca-nut is not only used as medicine,it is also daily food in Hainan and Hunan Province.However,especially after the cancer crisis of Areca-nut,the safety has became the focus in society.It is extremely easy to produce exogenous harmful substances during the processing of growth,collection,and storage,such as pesticide residues,mycotoxin and polycyclic aromatic hydrocarbons.However,the current existing quality standards and analysis methods are not able to meet the monitor requirements for the exogenous harmful residues in areca-nut.Therefore,it is necessary to study the quality control of areca-nut products in order to ensure the food safety.In this study,the analysis methods for benzoapyrene,four aflatoxins and nine organophosphorus pesticide residues in areca-nut were developed.Besides,extraction solvent,purification conditions and chromatographic conditions were investigated.One percent of acetic acid in acetonitrile was used as extraction solvent for the nine organophosphorus pesticide residues in areca-nut.After the extraction and dilution,it was analyzed by LC/MS/MS system.The quantitative ion pair of the nine organophosphorus pesticides were 303.0/145.1(methidathion),368.0/110.9(phosalone),318.0/160.0(phosmet),255.1/193.1(menite),306.1/108.0(pirimiphos-methyl),323.0/171.0(sulfotepp),258.9/127.1(dipterex),314.1/162.1(phentriazophos),142.0/94.0(methamidophos),respectively.The linear range was 2-20ng/mL,and the correlation coefficient r was above 0.999.Standard substances was added to the matrix of areca-nut for the recovery experiments.The average recovery was 73.4?120%,and RSD was 0.59-9.93%.The limit of detection(LOD)was 50.0?g/kg,which indicated that the methods could meet the analysis requirements of organophosphorus pesticide residues in areca-nut.A dispersive solid-phase extraction-liquid chromatography method was developed for the analysis of benzo(a)pyrene in edible areca-nut.The edible areca-nut samples were extracted by hexamethylene,and purified by PSA(N-propyl ethylenediamine)as sorbent,and then the concentration of benzo(a)pyrene was determined by high-performance liquid chromatography coupled with fluorescence detection.The linear range of benzo(?)pyrene was 2?20ng/mL,and the correlation coefficient r was 0.9997.By adding standard substance in the matrix of smoked and green areca-nuts,an average recovery of 83.0?114.5%was achieved,and the RSD was ranging from 1.27?6.78%.The limit of detection(LOD)was 1.0?g/kg.One percent of acetic acid in acetonitrile was used as the extraction solvent for the four kinds of aflatoxins residues(Bi,B2,Gi,G2).PSA powder(N-propyl ethylenediamine)was applied for sample purification,and then LC-MS/MS was used for the analysis.The quantitative ion pairs were 313.2/285.2(aflatoxinBi),315.2/287.2(aflatoxin B2),329.2/243.1(aflatoxin G1)331.2/245.1(aflatoxin G2),respectively.The linear range of these four aflatoxins was 0.1?10ng/mL,and the correlation coefficient r were all above 0.999.Standard substance was added to the matrix of areca-nut,and the average recovery was 80.0%?99,2%,and RSD was in the range of 1.49?9.26%.The limit of detection(LOD)was 1.0?g/kg.The developed methods were applied for the analysis of nine brands of areca-nut from markets in Haikou.Among these samples,no organophosphorus pesticides residue were detected,benzo(a)pyrene was detected in two sample(2.53?g/kg and 1.15?g/kg,respectively),and eaflatoxin B2 was detected in one sample(0.32?g/kg).The analytical methods of benzo(a)pyrene,aflatoxins and organophosphorus pesticide were validated and applied for the analysis of the residues in the areca-nut samples.The results showed that the pretreatment method is simple,accurate,and producible with a low limit of detection.It is a great method for determining exogenous harmful residues in areca-nuts from different production processes.