杀菌剂中抑霉唑含量的离子对高效液相色谱分析

Determination of Enilconazole in Germicide by Ion-pair High Performance Liquid Chromatography

选用庚烷磺酸钠作离子对试剂 ,拟定了杀菌剂中抑霉唑及其硫酸盐的反相离子对HPLC测定方法。讨论了离子对的形成过程 ,pH值对离子对形成的影响 ,推导了流动相pH值计算公式 ,估算了流动相的pH值范围 ,确定了色谱柱为EclipseXDB C815 0mm× 4 .6mm ,流动相为甲醇 :含 12mmol/L庚烷磺酸钠的 2 5mmol/L磷酸盐缓冲溶液 (pH≈ 2 .8) =6 2∶38(V/V) ,测定波长为 2 2 5nm的分析条件。方法的检出限为 7.1× 10 -4μg ;线性范围为 8.0× 10 -3 ～ 4 .0 μg ,实验结果线性关系良好 ;相关系数r =0 .9998。方法用于杀菌剂样中抑霉唑及其硫酸盐的测定 ,回收率 99.7% 。

A ion-pair high performance liquid chromatographic (HPLC) method for the determination of Enilconazole and enilconazole sulfate in germicide was developed. Effect of the acidity on formation of ion-pair associate of enilconazole with 1-Heptanesulfonate was discussed. The optimal scope of acidity was 2<pH<6 and chromatographic conditions were: the column:Eclipse XDB-C 8 (150 mm×4.6 mm), the mobile phase: mixture of methanol-25mmol/L phosphate buffer (pH≈2.8) containing 12 mmol/L Sodium 1-Heptanesulfonate (62∶38, volume ratio), the flow rate: 0.8ml/min, the detection wavelength: 225 nm, and the column temperature:30℃. The linear range and detectable limit were 8.0×10 -3～4.0 μg and 7.1×10 -4 μg respectively. The average recovery was 99.7% and RSD was low 0.5%. The method has proven to be much fast, simple, sensitive, accurate and reproducible than gas chromatographic method, reported already. The assay results can be used as a very important criterion for large-scale production.