篇名:
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Comparison of Ion-pairing and Ion-Suppressing Liquid Chromatographic Methods for the Determination of Pyrimethamine and Ormetoprim in Chicken Feed
作者:
林士鈺;鄭秀蓮
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 NaHOP4 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.
備註:
年份:西元 2003 年
期別:第 39 期
詳細內容:
Although pyrimethamine (PYR) can prevent leucocytozoonosis in chickens (1), it is not allowed to be used as feed additive (2,3). The problem of residual PYR in eggs has caused serious public concern since 1986 in Taiwan. Ormetoprim (OMT) is an analog of PYR and is permitted for use as feed additive for the prevention of leucocytozoonosis (2,3). The National Institute for Animal Health is responsible for the testing of PYR and OMT in feed; therefore, a simultaneous determination method for OMT and PYR is urgently needed.  Although spectrophotometry (4,5) and gas chromatography (6) have been used to determine PYR, high-performance liquid chromatography (HPLC) is the most frequently used method in monitoring PYR in edible tissues, plasma, and urine (7-16) and veterinary commercial formulations (17). The methods for determination of OMT are fluorospectrometry (18) and HPLC (19).  The determination of PYR by reversed-phase HPLC involves either ion-pairing chromatography (7,8,12) or ion-suppressing chromatography (9,10). In this study, these two methods are compared in order to choose the best analytical conditions, and a method for the simultaneous determination of OMT and PYR was developed.
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附件名稱:
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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