篇名:
配離子與抑制離子化液相色層分析法對雞飼料內必利美達民及歐美德普之比較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:
利用高效液相色層分析法(HPLC)同時檢驗雞飼料必利美達民(PYR) 及歐美德普(OMT)。以配離子HPLC分析PYR及OMT,其滯留常數(k’)於 有機相(acetonitrile)濃度之關係,呈一特殊線型。增加acetonitrile濃度時 k’值先下降而後緩慢上升,但acetonitrile濃度增至90%時則快速上升。當有機相 增加時,PYR及OMT之解析常數(Rs)緩慢降低。當配離子濃度增加時k’及 Rs值下降。於82% acetonitrile在0.005M PIC B-8可得最佳k’及Rs值。於抑制離子化HPLC,在pH 7.5時Na2HPO4之濃度對PYR或OMT之k’及Rs值影響 不大。但在pH 4.0時k’及Rs值下降。一般而言,配離子HPLC法較抑制離子 之PYR及OMT可呈線性關係。Sufamonomethoxine,sulfadimethoxine,sulfaquinoxaline,trimethoprim,amprolium,clopidol,and nicarbazin不會干擾PYR及OMT之檢出。飼料內1mg/kg及5mg/kg之PYR回收率分別為73.0%及72.0%,而3mg/kg及7mg/kg則分別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-paring 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 1-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 pH 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 the 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 2001 年
期別:第 37 期
詳細內容:
Although pyrimethamine (PYR) can prevent leucocyto- zoonosis in chickens (1), it is not allowed to be used as a 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 a 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 tissued, plasma, and urine (7-16) and veterinary commercial formulations (17). The methods for the 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:
配離子與抑制離子化液相色層分析法對雞飼料內必利美達及偶歐美德普之比較
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