| Fruit and fruit juice products are essential material sources for human life.In China,a large number of fruit and fruit juices are produced every year,but in the process of fruit and fruit juice production,the use of illegal pesticides and improper storage,transportation and processing have resulted in the excess of pesticide and fungin residues.The excess of mycotoxins and pesticide residues will be harmful to the health of human and livestock,and the export and circulation of fruit and fruit juice in China will be blocked.Therefore,it is necessary to establish a rapid,simple and sensitive method for the analysis of residue in fruit and fruit juice.In this paper,the residues of 10 kinds of mycotoxins[patulin(PAT),ochratoxin A(OTA),citrinin(CIT),aflatoxin B1(AF B1),aflatoxin B2(AF B2),aflatoxin G1(AF G1),aflatoxin G2(AF G2),alternariol(AOH)],alternariolmethyl ether(AME),tenuazonicacid(TeA),carbamate pesticides and organophosphorus pesticides were analyzed.Based on the dispersive liquid liquid microextraction,the acid assisted liquid microextraction and ultrasonic assisted solid-phase suspension dispersion liquid extraction were established.The main results are as follows:1.An acid-assisted liquid-liquid microextraction combined with liquid phase tandem mass spectrometry was established to determine OTA,CIT,AF B1,AF B2,AF G1,AF G2,AOH,AME residue in mango juice,pineapple juice and banana juice.The optimum conditions: the juice matrix 5 mL,the extractant is 3-chloroaniline,the dosage of extractant is 60 ?L dispersant is 1.5 mL of the hydrochloric acid of pH=0.4,the pH value of the system after the acid-base reaction is 5,the centrifugation time is 5 min,the fixed volume deposition phase to 200?L.Under the optimal conditions,The spiked levels of 8 target toxins were 0.2,1,10 ?g/L,the extraction recovery in mango juice was 75.6~103.4%,and the RSD was less than 14.2%.the method extraction recovery rate of 8 target toxins in pineapple juice was 77.2~107.1%,RSD was less than 15.5%,and the method extraction recovery rate of three different concentrations in the banana juice from the target toxin was 222.3%,232%,44.8%,indicating that the establishment of AME method in banana juice failed.The method extraction recovery rate of other toxins was 78.4%~123.7% and RSD was less than 17%.In addition to AME in banana,other targets have a linear range of 1~500 ?g/L,and the detection limit is 0.23~17.71 ng/L,which meets the requirement of target toxin detection in fruit juice.2.The optimum conditions for the extraction of carbamate and organophosphorus pesticides were obtained by using the established acid-assisted liquid-liquid microextraction.The pesticides(1.Aldicarb 2.Carbendazim 3.Chlorpyrifos-methyl 4.Dichlorvos 5.dimethoate 6.Edifenphos 7.Fenthion-sulfoxide 8.Isoprocarb 9.Malathion 10.Methomyl 11.Mocap 12.Pirimicarb 13.Tolclofos-methyl 14.Triazophos,respectively)in banana juice,apple juice and mango juice were established.The spiked levels of 14 target pesticides were 0.5 ?g/L,2.5 ?g/L and 10 ?g/L.The method extraction recovery rate in banana juice was 74.3~121.8%,RSD was less than 19.2%;the method extraction recovery rate in apple juice was 75.4~112.6%,RSD was less than 14.8%;the method extraction recovery rate in grape juice was 72.7~112.5%,and the RSD was less than 19.3%.The linear range of all targets is 0.5~100 ?g/L,and the detection limit is 0.46~106.76 ng/L,which meets the requirements of target pesticide detection in fruit juice.3.A method of ultrasonic-assisted solid-phase suspension dispersion liquid-liquid microextraction combined with liquid phase tandem mass spectrometry was established to determine the residues of 4 toxins such as OTA,CIT,AME and AOH in mango juice,fire dragon juice and lychee juice.The optimum conditions are as follows: the juice matrix 5mL,pH=3,the extractant are 1-dodecanol,the dosage of extractant is 40 ?L,the dispersant is 1 mL of ethanol,and the fixed volume is mixed with the 10 ?L of upper liquid and 90 ?L acetonitrile.The spiked levels of 4 target mycotoxins were 0.2,1,10 ?g/L,the method extraction recovery rate in mango juice was 88.7~110.1%,the RSD was less than 13.3%,the method extraction recovery rate in the fire dragon juice was 77.4~123.0%,the RSD was less than 14.8%,the method extraction recovery rate in the lychee juice was 86.1~109.0%,and the RSD was less than 11.1%.The linear range of all targets is 0.5~100 ?g/L,and the detection limit(LOD)is 0.46~106.76 ng/L,which meets the requirement of target toxin detection in fruit juice.4.The optimum conditions for the extraction of carbamate and organophosphorus pesticides were obtained by using the ultrasonic-assisted solid-phase suspension dispersion liquid microextraction.The pesticides in apple juice,grape juice and banana juice were established(1.Carbendazim 2.Chlorpyrifos-methyl 3.Edifenphos 4.Mocap 5.Isoprocarb 6.Malathion 7.Phoxim 8.Tolclofos-methyl 9.Triazaphos).The spiked levels of 9 target pesticides were 0.5,2.5 and 10 ?g/L.The method extraction recovery rate in apple juice was 75.7~112.3%,and the RSD was less than 16.4%;the method extraction recovery rate in grape juice was 78.5~118.0%,RSD was less than 19.5%;the method extraction recovery rate in banana juice was 72.4~112.0%,and RSD less than 17.6%.The linear range of all targets is 1~200 ?g/L,and the detection limit is 0.28~88.5 ng/L,which meets the requirements of target pesticide detection in fruit juice. |
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