高效液相色谱法定量测定1,3-二甲基-5-吡唑酮的方法建立

The Method of Quantitative Determination of 1,3-dimethyl-5-pyrazolone by High Performance Liquid Chromatography

[目的]建立用于鉴别及测定1,3-二甲基-5-吡唑酮(DP)的高效液相色谱(HPLC)方法。[方法]采用高效液相色谱仪定量测定DP,对其色谱条件进行优化。[结果]测定DP的最佳色谱条件如下:色谱柱Diamonsil-C18(2)(250.0 mm×4.6 mm×5μm),甲醇和水为流动相,DAD检测器,检测波长为242 nm,流速为0.4 ml/min,柱温35℃。在上述条件下,DP得到很好的分离,在给定的浓度范围内呈现良好的线性相关(r2>0.999),精密度良好,回收率为98.74%,相对标准偏差为1.6%。[结论]该方法具有良好的灵敏度、回收率和重复性,可用于DP的鉴别及测定。

ZHANG Li-jie, WENG Ting, LIU Zhi-yong, SUN Ya-quan. （ 1. Nanjing University of Technology, Nanjing, Jiangsu 210000; 2. Yancheng Teachers University, Yancheng, Jiangsu 224051 ;3. Sword Pesticides Company, Yanebeng, Jiangsu 224799 ;4. Marine Organisms Pharmacentical Limited Company,Dafeng Yangcheng Teachers College,Dafeng,Jiangsu 224100） Abstract [ Objective ] The aim was to establish a method of quantitative determination of 1,3-dimethyl-5-pyrazolone by high performance liquid chromatography. [ Method] The reversed phase high performance liquid chromatography （HPLC） was applied to identification and determination of DP. [ Result ] SHIMADZU SPD-20A system equipped with on line degasser was used, Diamonsil reversed phase-C18 （2） （250.0 mm × 4.6 mm ×5 μm） column as stationary phase, methyl alcohol and water as mobile phase. The flow rate was 0.4 ml/min; the column temperature was 35 ℃ ; and the detection wavelength was 242 nm. DP had a good resolution within 10 min. In the given concentration range, DP presented good linear correlation （r^2 〉0. 999） ; the recovery rate was 98.74% ,and the RSD of repeatability was 1.6%. [ Conclusion] The sensitivity,recovery and repeatability of this method are good. This method can be used for the identification and determination of DP.