超高效液相色谱法应用于利福平胶囊的检验效果

Test effect of ultra-high performance liquid chromatography on Rifampicin capsules

目的探讨超高效液相色谱法应用于利福平药物的检验效果。方法选取利福平胶囊1瓶(100粒)作为供试品,依法进行样品制备,A组和B组各10粒,在利福平药物检验中分别应用高效液相色谱法和超高效液相色谱法。A组色谱条件:色谱柱Kromasil C_(8)柱(5μm,4.6 mm×150.0 mm),色谱柱Inertsil■柱(5μm,4.6 mm×150.0 mm),流动相为甲醇-乙腈-0.075 mol/L磷酸二氢钾溶液-1.0 mol/L枸橼酸溶液(30∶30∶36∶4),流速为1.0 ml/min。B组色谱条件:色谱柱Kromasil C_(8)柱(3.5μm,4.6 mm×50.0 mm),色谱柱Inertsil■柱(5μm,2.7 mm×50.0 mm),流动相为甲醇-乙腈-0.075 mol/L磷酸二氢钾溶液-1.0 mol/L枸橼酸溶液(30∶30∶36∶4),流速为1.0 ml/min。两组供试品溶液制取方法一致。A组取经0.45μm微孔滤膜过滤的溶液,置紫外线200~400 nm范围内进行波长扫描,末端吸收210/220 nm,最后确定测定波长,并精密吸取滤液10μl注入到常规液相色谱仪中;B组取经0.45μm微孔滤膜滤过后溶液,精密吸取滤液10μl注入到超高效液相色谱仪中。比较两组利福平药物在不同检验方法下的药物分析时间和分离度。结果B组在柱温25℃时药物分析时间为(6.44±0.40)min,柱温35℃时药物分析时间为(1.28±0.16)min,均低于A组的(18.49±3.18)、(14.25±2.73)min,差异有统计学意义(P<0.05)。B组在柱温25℃时药物彻底分离率为98.00%,柱温35℃时药物彻底分离率为100.00%,均高于A组的84.00%、88.00%,差异有统计学意义(P<0.05)。结论超高效液相色谱法应用于利福平药物检验效果显著优于高效液相色谱法,超高效液相色谱法应用后利福平药物检验平均分析时间显著缩短、药物分离效果更高,因此该方法在利福平药物检验中的应用更具推广价值。

Objective To investigate the effect of ultra-high performance liquid chromatography in the test of Rifampicin.Methods One bottle of Rifampicin capsules(100 capsules)was selected as the test product,and samples were prepared according to law,with 10 capsules in group A and 10 capsules in group B.high performance liquid chromatography and ultra-high performance liquid chromatography were used in rifampicin drug testing,respectively.Chromatographic conditions of group A:chromatographic column Kromasil C_(8)(5μm,4.6 mm×150.0 mm),Inertsil■(5μm,4.6 mm×150.0 mm),the mobile phase consisted of methanol-acetonitrile-0.075 mol/L potassium dihydrogen phosphate solution-1.0 mol/L citrate solution(30∶30∶36∶4)at a flow rate of 1.0 ml/min.Chromatographic conditions of group B:chromatographic column Kromasil C_(8)(3.5μm,4.6 mm×50.0 mm),Inertsil■(5μm,2.7 mm×50.0 mm),the mobile phase consisted of methanol-acetonitrile-0.075 mol/L potassium dihydrogen phosphate solution-1.0 mol/L citrate solution(30∶30∶36∶4)at a flow rate of 1.0 ml/min.The preparation methods of the two groups of test solutions are the same.Group A takes the solution filtered by a 0.45μm microporous membrane,and scans the wavelength within the range of 200-400 nm of ultraviolet light.The end absorbs 210/220 nm,and finally determines the measurement wavelength and accurately absorbs the filtrate.10μl was injected into a conventional liquid chromatograph.Group B took the solution filtered through a 0.45μm microporous membrane,and precisely aspirated 10μl of the filtrate and injected it into an ultra-high performance liquid chromatograph.The drug analysis time and separation degree of Rifampicin were compared between the two groups under different testing methods.Results The drug analysis time in group B was(6.44±0.40)min at column temperature 25℃,(1.28±0.16)min at column temperature 35℃,which were lower than those in group A(18.49±3.18)and(14.25±2.73)min,and the differences were statistically significant(P<0.05).The complete drug separation rates of group B at 25℃and 35℃were 98.00%and 100.00%,which were higher than those of group A(84.00%and 88.00%),and the differences were statistically significant(P<0.05).Conclusion The effect of ultra-high performance liquid chromatography applied to rifampicin drug testing is significantly better than that of high performance liquid chromatography.The application of the method in the drug testing of rifampicin has more promotion value.