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제안 방법
- Standard solutions were injected into an LC column and peak areas were measured to calculate streptomycin residue concentrations. A calibration curve was generated by plotting the concentrations of the injected standards versus the peak areas observed and the linearity of this method was evaluated by analyzing 5 working solutions. The peak areas obtained with different streptomycin concentrations were used to calculate the residue concentrations (R2 = 0.
- The ratio of the areas of the most intensive product ions of streptomycin (m/z 263) was used for quantification. Calculations of the concentrations of the spiked samples for the determination of recovery were performed using matrix calibration curves that included 5 concentration levels. These matrix calibration samples were spiked with the working solution.
- Recovery studies were done using 0.01, 0.05, and 0.5 ㎎/㎏ fortification levels for streptomycin in blank kiwifruit (Fig. 3). The recovery data and the relative standard deviations obtained by this method are summarized in Table 3.
- The specificity of the method was evaluated by injecting a procedural blank, kiwifruit blank samples, and blank samples spiked with the lowest fortification level assayed. The accuracy of the method was determined by a recovery test using samples spiked with 3 concentration levels of streptomycin: 0.01, 0.05, and 0.5 ㎎/㎏.
- These were prepared by diluting the stock solution. The specificity of the method was evaluated by injecting a procedural blank, kiwifruit blank samples, and blank samples spiked with the lowest fortification level assayed. The accuracy of the method was determined by a recovery test using samples spiked with 3 concentration levels of streptomycin: 0.
- Therefore, in this study, we developed and validated an analytical method to determine streptomycin residues in kiwifruit samples.
대상 데이터
- For operation in the MS/MS mode, the collision gas was argon (99.999%) with a pressure of 1.2 × 10−3 mbar in the collision cell. Capillary and extractor voltages of 1 kV and 5 voltage (V), respectively, were used in the positive ionization mode.
- LC grade water was obtained by purifying distilled water in a high performance reverse osmosis (RO) system (Sartorius Stedim Biotech, Göttingen, Germany). HPLC grade formic acid was purchased from Sigma-Aldrich. GHP syringe filters (0.
- Recovery experiments used 6 replicates for each of these concentrations. Precision was evaluated within the same day at each recovery level and was determined as the relative standard deviation (RSD) for 6 replicates.
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