| The full automatic TurboFlow online solid phase extraction (TurboFlow online SPE) is an sample preparation technique developed in recent years. The sample matrix was eliminated and the targets were acquired at the same time with TurboFlow online SPE which combined eddy diffusion with chemical action by using large sized bonded phases as filler. Coupling to TurboFlow online SPE, the speed, accuracy, and automation of chromatography were improved significantly. With the further study, TurboFlow online SPE was applied to bioanalysis and environmental monitoring, but its application in food safety was infrequent. The application of TurboFlow online SPE in determination of drug residues in animal products was studied systematically in this paper. A series of analytical methods were developed by optimizing online purification parameters, chromatographic conditions, and mass spectrometric parameters for the detection of antiviral drugs in chicken, antibiotics in milk, and β-agonists. These rapid methods are necessary to ensure food safety, strengthen market management and answer technological barriers in the international trade. The research contents include three partials which were discussed as follows.1A simple and rapid method using fully automatic TurboFlow online solid phase extraction (TurboFlow online SPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for simultaneous analysis of amantadine and moroxydine. The target compounds were extracted from chicken with1%acetic acid acetonitrile (ACN)-water (4:6, v:v) and purified on Cyclone TurboFlow online column by increasing the retention of moroxytion with sodium heptanesulfonate(HPSF-Na). The separation was carried out on a CAPCELL PAK CR (1:4) column with the interaction of both hydrophobic interaction and strong cation exchange, and the detection was performed with tandem mass spectrometry in selected reaction monitoring (SRM) mode. The effects of extraction condition, purification parameters, and detection conditions were investigated in this study. Using the optimized conditions, the linear range of analytes was from0.4to100μ/kg. The limits of quantification (LODs) of amantadine and moroxydine were0.25and0.30μg/kg respectively, and LOQs were both1.0μg/kg. The recoveries were between73.2%and109.8%, with the relative standard deviations (RSDs) in the range of3.8%-9.0%. The validation results indicated that the sensitive and accurate method can be applied to the routine laboratory analysis of large numbers of samples.2An online analysis method has been firstly established for simultaneous determination of88veterinary drugs (VDs) in milk. The analytes were released and extracted with acetonitrile followed by purified with Cyclone column, separated with MG Ⅲ column and detected with MS/MS in SRM mode. The influences of different experimental parameters including extraction, purification, separation, and detection were studied separately in this experiment. Under the optimized conditions, the developed method was validated and good performance characteristics were obtained. The linear regression coefficients (R) of matrix-match calibration standard curves established for quantification were all higher than0.99. The LOQs of all target compounds ranged from1to20μg/kg. Average recoveries were between62.5%and133.5%, with the RSDs in the range of6.2%～30.8%. The results indicated clearly that the developed method was rapid and accurate, and can be applied to the routine laboratory analysis of large numbers of samples frequently measureing different classes of compounds.3Online determination of11(3-agonists in urines was developed by using TurborFlow online SPE-LC-MS/MS. The urines were cleaned up with MCX TurboFlow column for the first time. The urines were cleaned up with MCX column. Followed the elution with methanol (containing5%ammonia):water (8:2, v:v), the analytes were separated with C18column and detected with MS/MS in SRM mode. The optimization and validation were performed in this section. Under the optimized conditions, the LODs and LOQs were in the range of0.05～0.5μg/kg and0.11.0μg/kg, and the recoveries were from75.2%to109.0%with RSDs (n=10) between4.3%and16.1%. The application of57urines demonstrated the sensitive, accurate, and rapid method fulfilled the requirement of determination and was applicable to the determination and screening of large batch urines. |
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