The Research Of Clove Phenol Drug Residue Detection In The Aquatic Products

An experiment was conducted with the aquaculture products(tilapia,vannamei,et) to establish the HPLC method for determining five kinds of eugenol drug residues, Eugenol,iso-eugenol, Methyl eugenol,Methyl iso-eugenol,Acet-yl iso-eugenol through the research to optimize sample preparation method, chromatographic conditions and MS conditions.And it also established the gas chromatography and the gas chromatography-mass spectrometry methods, for the detection of six kinds of eugenol drug residues,Eugenol,Methyl eugenol, Iso-eugenol, Methyl iso-eugenol, Eugenol acetate, Acetyl iso-eug enol in aquatic products at the same time. The main research contents and results are as follows:1. Detectionation of five kinds of clove phenol drug residue in Aquatic Products by HPLC methods.A high performance liquid chromatography(HPLC)method has been developed for the detection of five kinds of eugenol,drug residues Eugenol,Iso-eugenol,Methyl eugenol,Methyl iso-eugenol,Acetyl iso-eugenol in aquatic products at the same time.Sample was ultrasonic extracted by acetonitrile,and the fat was cleaned up twice by n-hexane and then the diluted solution was determined by HPLC. External standard calibration was adopted in the determination. Five kinds of eugenol type of anesthetic showed good linearity in the concentrations range of 0.05~10.00 μg/mL for the standard solutions carves,and all of the correlation coefficents(R2) were higher than 0.9990. At the spiked levels of 0.10~1.00 mg/kg,the average recoveries were 80.76%~102.63%. The relative standard deviations were 0.25%~5.49%. The limits of quantificationg of Eugenol,Iso-eugenol and Methyl iso-eugeno were 0.05mg/kg,and Methyl eugenol and Acetyl iso-eugenol were 0.10 mg/kg.2. Detectionation of six kinds of clove phenol drug residue in Aquatic Products by GC methods.A dispersive solid-phase extraction-gas chromatography(GC)method has been developed for the detection of six kinds of eugenol drug residues in aquatic products at the same time. Sample was ultrasonic extracted by acetone,Constant volume after rotary evaporation concentration,using dispersive solid-phase extraction(DSPE) purification,determined by gas chromatograph. External standard calibration was adopted in the determination. Six kinds of eugenol type of anesthetic showed good linearity in the concentrations range of 0.05~10.0 μg/mL for the standard solutions carves,and all of the correlation coefficents(R2) were in 0.9995~0.9999. At the spiked levels of 0.1~1.0 mg/kg in blank musclesample,the average recoveries were 80.3%~103.2%.The relative standard deviations were 0.7%~5.4%. The limits of quantificationg(LOQ),all of the six kinds of eugenol drug residues(Eugenol,Methyl eugenol,Iso-eugenol,Methyl iso-eugenol,Eugenol acetate,Acetyl iso-eugenol)were 0.1 mg/kg.3. Detectionation of six kinds of clove phenol drug residue in Aquatic Products by GC-MS methods.A gas chromatography-mass spectrometry(GC-MS)method has been developed for the detection of six kinds of eugenol drug residues in aquatic products at the same time.Sample was ultrasonic extracted by acetonitrile,using dispersive solid-phase extraction(DSPE)purification and then drying by nitrogen,volume constanted with acetone,determined by gas chromatograph-mass spectrometry. External standard calibration was adopted in the determination. Six kinds of eugenol type of anesthetic showed good linearity in the concentrations range of 1.0~200.0 μg/L for the standard solutions carves,and all of the correlation coefficents(R2) were in 0.9956~0.9995. At the spiked levels of 1.0~10.0 μg/kg in blank muscle sample, the average recoveries were82.2%~100.7%.The relative standard deviations were 0.6%~7.4%. The limits of quantificationg(LOQ), Eugenol, Methyleugenol, Iso-eugenol and Acetyl iso-eugenol were1.0 μg/kg,and Methyl iso-eugenol, Eugenol acetate were 0.5 μg/kg.