复硝酚钠原药中3种有效成分的高效液相色谱分析

Analysis of three compounds of sodium nitrophenolate TC by high performance liquid chromatography

建立了快速、可同时测定复硝酚钠原药中5-硝基-2-甲氧基苯酚钠(SD1)、二水合4-硝基苯酚钠(SD2)和2-硝基苯酚钠(SD3)3种有效成分的高效液相色谱(HPLC)分析方法。通过对流动相和检测波长的优化,得到3种成分的最佳色谱体系。采用Eclipse XDB C18色谱柱(250 mm×4.6 mm,5μm),以V(甲醇)∶V(水)=60∶40为流动相进行洗脱,流速1.0 mL/min,柱温30℃,在335 nm波长下,3种有效成分在7 min内能达到基线分离。SD1、SD2和SD3的峰纯度因子均大于999;线性范围分别为0.6～286.7、0.5～518.5和0.5～272.0 mg/L,相关系数r均大于0.999;定量限(LOQ)分别为0.6、0.5和0.5 mg/L;其质量分数分别为15.8%、50.0%和33.0%,标准偏差分别为1.7%、1.0%和1.3%。该方法可在较短时间内使在色谱柱上不易保留和分离的复硝酚钠中的3种组分同时分离,操作简单、快捷,结果准确、可靠,为复硝酚钠原药的质量控制提供了一种准确可行的分析方法。

A rapid high performance liquid chromatography （HPLC） method for simultaneous determination of sodium 5-nitroguaiacolate（ SD1 ）, sodium 4-nitrophenoxide dihydrate （SD2） and sodium 2-nitrophenoxide（ SD3 ） in compound sodium nitrophenolate technical material（TC） was established. The optimum chromatographic conditions have been set up after examing the mobile phase and the detector wavelength. The determination was carried out on a Eclipse XDB C18 column （250 mm ~4.6 mm,5 p^m） with mobile phase V（ methanol）： V（water） = 60： 40, detection wavelength 335 nm,column temperature 30 ~C and flow rate 1.0 mL/min. Complete separation of the above three comounds was achieved in 7.0 rain under the optimized conditions. The developed method was fully validated. The peak purity factor of sodium 5-nitroguaiacolate, sodium 4-nitrophenoxide dihydrate and sodium 2-nitrophenoxide were all above 999 and the linear ranges were 0.6 -286.7 mg/L,0.5 -518.5 mg/L and 0.5 -272.0 mg/L,respectively, with their correlation coefficients greater than 0. 999. The limit of quantitation （ LOQ ） were 0.6,0. 5 and 0.5 mg/L. The contents of the three compositions were 15. 8%, 50.0% and 33.0%, with their relative standard deviations 1.7%, 1.0% and 1.3 %, respectively. The optimized and validated method is efficient, accurate and easy to use, which provides theory basis and reliable method for determination and quality control of compound sodium nitrophenolate TC.