高效毛细管电泳法同时检测地克珠利和妥曲珠利的含量

Simultaneous Determination of Diclazuril and Toltrazuril by High-Performance Capillary Electrophoresis

关键词:  地克珠利，妥曲珠利，高效毛细管电泳

Key words:  Diclazuril  Toltrazuril  High-Performance Capillary Electrophoresis

摘要:

采用毛细管电泳-二极管阵列检测法建立了地克珠利和妥曲珠利两种结构相近的均三嗪类抗球虫药物的分离检测方法。未涂层石英毛细管柱(75µm×50cm)，采用0.5 psi压力进样6s，分离电压为22kV，柱温为20℃，紫外检测波长210nm；运行缓冲液为30mmol•L-1硼砂缓冲液(用30mmol•L-1 NaOH调至pH9.5)。探讨了缓冲溶液的种类、浓度、pH等诸因素对分离检测结果的影响。上述2种药物在8min内实现了基线分离。线性检测范围为0.5～100µg•L-1，检出限为0.1µg•L-1 (S/N=3)。应用于市售妥曲珠利溶液的含量测定，取得满意结果。

Abstract:

A capillary electrophoresis (CE) method with PAD detection has developed for analysis of diclazuril and toltrazuril. In this experiment, we have considered the experimental conditions, such as the injection pressure, separation voltage, injection time, temperature, pH, and ions concentration of the separation buffer in detail. Under the optimal chromatographic condition, the diclazuril and toltrazuril were performed on an automated CE system (P/ACE MDQ, Beckman, Fullton, CA), with PAD detection at 210 nm. Data were collected and analyzed on System 32 Kata Software. A fused-silica capillary was used, 60cm in total length (50cm to the detector) and 75µm internal diameter (i.d.). The samples were loaded with an argon pressure injection at the positive end (anode) and detection at the negative end (cathode), Running buffer solutions was 30mmol•L-1 sodium borate (30mmol•L-1 NaOH adjust to pH9.5)and the column temperature was maintained at 20 ℃. The retention time of DIC and TOL are respectively 7.39min and 7.14mim.The suitability of method for quantitative determination was approved through validation specification, such as linearity, precision, accuracy, limit of detection and quantification.