摘要
建立了高效液相色谱法(HPLC)测定兽用除虫脲原料药含量及有关杂质的检测方法。采用C18色谱柱(250 mm×4.6 mm,5μm),以甲醇为流动相A,0.01 mol/L乙酸铵溶液为流动相B,进行梯度洗脱,流速1.0 mL/min,检测波长254 nm,进样量10μL,柱温25℃。除虫脲的线性范围为10~1000μg/mL(R 2=0.999),回收率97.01%~100.83%(RSD<1.0%,n=3),精密度(RSD=0.13%,n=9)、重复性(RSD=0.45%,n=6)良好,主成分与各杂质峰分离良好。以主成分自身对照法计算,各杂质峰面积的和不得大于对照溶液主峰面积的0.1倍(0.1%)。该方法简便灵敏,结果准确可靠,可作兽用除虫脲原料药含量及有关杂质测定。
A method based on HPLC was developed for determination of the content and related substances of veterinary diflubenzuron.Using C18 column(250 mm x 4.6 mm,5μm)and methanol as mobile phase A,0.01 mol/L ammonium acetate solution as mobile phase B,with gradient elution.The flow rate was 1.0 mL/min.The UV detection at 254 nm.The injection volume was 10μL.The column temperature was 25℃.The results showed that linear range of the method was 10~1000μg/mL(R 2=0.999),the recovery rate of the preparation was between 97.01%and 100.83%(RSD<1.0%,n=3),with good precision(RSD=0.13%,n=9)and repeatability(RSD=0.45%,n=6).The main component and impurities could achieve a good separation.Calculated by the main component self-control method,the sum area of each impurity peak was not more than 0.1 times(0.1%)of the peak area of diflubenzuron in the control solution.This method was simple,sensitive,accurate and can be used for the determination of content and related impurities of veterinary diflubenzuron raw materials.
作者
左三龄
张博
邱银生
叶纯
吴仲元
ZUO San-ling;ZHANG Bo;QIU Yin-sheng;YE Chun;WU Zhong-yuan(College of Animal Science and Nutritional Engineering,Wuhan Polytechnic University,Wuhan 430023,China)
出处
《中国兽药杂志》
2020年第2期46-52,共7页
Chinese Journal of Veterinary Drug
