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- Comparison of Ion-Pairing and Ion-Suppressing Liquid Chromatographic Methods for the Determination of Pyrimethamine and Ormetoprim in Chicken Food
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題名 | Comparison of Ion-Pairing and Ion-Suppressing Liquid Chromatographic Methods for the Determination of Pyrimethamine and Ormetoprim in Chicken Food=離子配液相層析法及抑制離子化層析法對飼料內必利美達民及歐美德普測定之比較 |
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作者 | 林士鈺; 鄭秀蓮; | 書刊名 | 行政院農業委員會家畜衛生試驗所研究報告 |
卷期 | 39 民92 |
頁次 | 頁53-59 |
分類號 | 437.714 |
關鍵詞 | 離子配液相層析法; 抑制離子化層析法; 雞; 飼料; 必利美達民; 歐美德普; Ion-pairing liquid chromatographic method; Ion-suppressing liquid chromatographic method; Pyrimethamine; Ormetoprim; Chicken food; |
語文 | 英文(English) |
中文摘要 | 為檢驗飼料內必利美達民(pyrimethamine, PYR)及歐美德普(Ormetoprim, OMT),乃開發高效液相層析法(High performance liquid chromatography, HPLC)。HPLC之離子配層析法中,當有機相Acetonitrile濃度增加時,容積因素(Capacity factor,K')降低,爾後緩慢升高,至90%,卻急速上升,而呈特殊之曲線,PYR及OMT均有相似之結果。解析力(Resolutions, Rs)卻因增加有機相濃度而持續下降。配離子PICB-8的濃度增加則PYR及OMT之K及Rs均降低。故以Acetonitrile:0.005M PICB-8=82:18可得最佳之K'及Rs。HPLC之抑制離子化層析法中,當pH7.5時,Na₂HPO₄濃度對PYR及OMT之K'及Rs的影響均甚微。但在pH4.0時,Na₂HPO₄濃度提高則K'及Rs均下降。比較上述二種方法,以前者較佳,故以Acetonitrile:H₂O =82:18內含0.001M PICB-8當作移動相。1-5mg/L之PYR及OMT可得線性良好之檢量線。Sufamonomethoxine、Sulfadimethoxine、Sulfaquinoxaline、Trimethoprim、Amprolium、Clopidol及Nicarbazin均不會干擾OMT及PYR之檢測。添加1mg/L及5mg/L PYT飼料之回收率為73.0%及72.0%,而3 mg/L及7 mg/L OMT則為50.3%及53.6%。 |
英文摘要 | A high-performance liquid chromatographic (HPLC) method is developed to simultaneously determine pyrimethamine (PYR) and ormetoprim (OMT) in chicken feed. In the Ion-pairing HPLC determination of PYR and OMT, the relation between the retention factor (k') and the concentration of the organic phase (acetonitrile) shows a characteristic curve. The k' value first decreases and then increases slowly with increasing concentrations of acetonitrile, but then increases rapidly when the acetonitrile concentration increases to 90%. Resolutions (Rs) of PYR and OMT decrease gradually when the concentration of organic phase increases. Increasing the concentration of the pairing ion sodium I-octanesulfonate (PIC B-8) can decrease the k' and Rs values. Optimum values of k' and Rs are obtained using 82% acetonitrile in 0.005M PIC B-8. IN ion-suppressing HPLC, varying the concentration of Na₂HPO₄ has little effect on either the k' or Rs values of PYR or OMT at 7.5. However at pH 4.0, k' and Rs decline when the concentration of Na₂HPO₄ increases. In general ion-pairing HPLC generates more satisfactory results than ion- suppressing HPLC. Using 82% acetonitrile in water containing 0.001M PIC B-8 as the mobile phase, linear calibration curves are obtained in range from 1 to 5 mg/L of PYR and OMT. Sulfamonomethoxine, sulfadimethoxine, sulfaquinoxaline, trimethoprim, amprolium, clopidol, and nicarbazin do not interfere with the detection of PYR or OMT. The recoveries of PYR from spiked feed at 1 and 5 mg/Kg are 73.0% and 72.0%, respectively, and those of OMT from spiked feed at 3 and 7 mg/Kg are 50.3% and 53.6%, respectively. |
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