氯霉素甲硝唑洗鼻剂的含量测定及其2-甲基-5-硝基咪唑的定量检查

目的建立高效液相色谱法测定氯霉素甲硝唑洗鼻剂中氯霉素、甲硝唑含量测定方法及其有关物质2-甲基-5-硝基咪唑的定量检查方法。方法采用高效液相色谱法。IntersilC18分析色谱柱（4.6mm×250mm,5μm）,流动相：甲醇-水（36∶64,含1%磷酸二氢钠,0.005mol.L-1十二烷基磺酸钠,磷酸调pH值3.0）,流速：1ml/min,检测波长310nm。结果2-甲基-5-硝基咪唑、甲硝唑和氯霉素理论板数分别约为4300、3700和3500,回归方程分别为：Y=0.0003191X-0.000003240（r=0.9993）,Y=0.000001435X-13.64（r=0.9997）和Y=0.000008098X-22.71（r=0.9998）;线性范围分别为0.0005700～0.002280μg;0.4230～2.115μg和0.4500～2.250μg;平均回收率分别为98.7%、100.3%、98.4%,RSD分别为2.4%、1.6%、1.2%;检测限分别约为0.0001、0.003、0.03μg。结论用高效液相色谱法同时测定氯霉素甲硝唑洗鼻剂中氯霉素、甲硝唑及其有关物质2-甲基-5-硝基咪唑的含量,操作简便,结果准确。

HPLC Determination of Metronidazole Chloramphenicol and 2-Methyl-5-nitroimidazole in Metronidazole Chloramphenico Collunarium

Aim To establish a method for detecting Chloramphenicol, Metronidazole and 2-Methyl-5-nitroimidazole in Collunarium by means of HPLC. Methods The chromatographic conditions include the Intersil C18 column and a mobile phase consisting of methanol-water （36： 64, containing 1% NaH2PO4, 0.005mol·L^-1 Sodium dodecylsulfonate, to regulate pH to 3.0 with phosphoric acid）. The flow rate was 1.0ml/min. The detection wavelength was 310nm performed at room temperature. Results The number of theoretical plates calculated by 2-Methyl-5-nitroimidazole , metronidazole and chloramphenicol peak were 4 300,3 700 and 3 500 respectively ; the regression equation was Y =0.0 003 19IX-0.000 003 240（ r =0.999 3） ,Y =0.000 001 435X-13.64（ r =0.999 7） and Y = 0. 000 008 098X - 22.71 （ r = 0. 999 8 ） respectively ; the linear range was 0.0 005 700 - 0. 002 280 μg ,0.4 230 -2. 115μg,0.450 0 -2.250 0μg respectively;the average recovery（ RSD ）was 98.7% （2.4）, 100.3% （ 1.6）, 98.4% （1.2） respectively ;the measurable lowest limit was 0.000 1,0.003, 0.03μg respectively. Conclusions The method is rapid, accurate and reliable.