HPLC梯度洗脱法同时测定美辛唑酮红古豆醇酯栓两组份的含量

Simutaneous Determination of Two Components of Indometacin,Furazolidone and Cuscohygrinolisα-Acetylbenzoacetate Suppositories by HPLCgradient Elution

目的:建立同时测定美辛唑酮红古豆醇酯栓中呋喃唑酮和吲哚美辛含量的HPLC分析方法。方法:采用Kromasil C 18色谱柱(250mm×4.6mm,5μm),以甲醇和0.02mol·L^(-1)磷酸二氢钾溶液(加三乙胺调节pH至5.7)为流动相进行梯度洗脱,流速1.0mL·min^(-1),检测波长为258nm,柱温30℃,进样量20μL。结果:呋喃唑酮和吲哚美辛的分离度良好;呋喃唑酮线性范围为5.64~67.63μg·mL^(-1)(r=1.0000),检测限为:0.04μg·mL^(-1),定量限为0.13μg·mL^(-1),平均回收率为99.2%(RSD=1.2%,n=9);吲哚美辛线性范围为4.23~50.74μg·mL^(-1)(r=1.0000),检测限为0.06μg·mL^(-1);定量限为0.22μg·mL^(-1),平均回收率为100.6%(RSD=0.9%,n=9)。结论:该检验方法准确、重复性好、专属性强,为美辛唑酮红古豆醇酯栓提升含量测定的检测方法提供了可靠参考。

Objective:To establish a HPLC method for the simultaneous determination of furazolidone and indomethacin in metazolidone suppositorium.Methods:A Kromasil C18 column(250mm×4.6mm,5μm)was used for gradient elution with methanol and 0.02 mol·L^(-1) potassium dihydrogen phosphate solution(adjusted pH to 5.7 by adding triethylamine)as mobile phases.The flow rate was 1.0 mL·min^(-1).The detection wavelength was set at 258nm,column temperature was 30℃,and sample size was 20μL.Results:The separation degree of furazolidone and indomethacin was good.The linear range of furazolidone was 5.64~67.63μg·mL^(-1)(r=1.0000).The limits of detection and limits of quantification were 0.04μg·mL^(-1) and 0.13μg·mL^(-1).The average recovery was 99.2%(RSD=1.2%,n=9).The linear range of indomethacin was 4.23~50.74μg·mL^(-1)(r=1.0000),and the detection limit was 0.06μg·mL^(-1).The limit of quantitation was 0.22μg·mL^(-1),and the average recovery was 100.6%(RSD=0.9%,n=9).Conclusions:The method is accurate,reproducible and specific,and provides a reliable reference for the determination of the content of methazolidone glycol ester suppositorium.