一测多评法测定山荷降脂粉中4种成分的含量

Determination of four components in Shanhe Lipid-Lowering Powder by quantitative analysis of multi-components by single marker

目的建立一测多评法测定山荷降脂粉中4种成分的含量的测定方法 ,并验证该方法的准确性和可行性。方法采用高效液相色谱法测定山荷降脂粉中4种成分的含量,色谱柱:Kromstar^(TM) C_(18)(4.6 mm×250 mm,5μm),流动相:乙腈(A)-0.4%磷酸水溶液(B),梯度洗脱,流速:0.8 mL/min,柱温:25℃,芥子碱硫氰酸盐、金丝桃苷、槲皮素、山奈酚的检测波长分别为330、354、375、363 nm,进样量10μL。以槲皮素为内标物,建立槲皮素与芥子碱硫氰酸盐、金丝桃苷、山奈酚的相对校正因子,并计算4种成分的含量,实现一测多评;同时采用外标法测定该4种成分的含量,比较计算值与实测值的差异,以验证一测多评法的准确性和可行性。结果芥子碱硫氰酸盐、金丝桃苷、槲皮素、山奈酚的平均回收率分别为1.21%、1.08%、0.94%、1.33%,槲皮素与芥子碱硫氰酸盐、金丝桃苷、山奈酚的平均相对校正因子分别为1.23%、0.53%、1.41%,3批山荷降脂粉中4种成分的计算值与实测值间差异无统计学意义(P> 0.05)。结论一测多评法测定山荷降脂粉中4种成分准确可行,对山荷降脂粉质量控制具有指导意义。

Objective To establish a method for the determination of four constituents in Shanhe Jiangzhi Powder by quantitative analysis of multi-components by single marker, and to verify the accuracy and feasibility of the method. Methods The contents of four components in Shanhe Jiangzhi powder were determined by high performance liquid chromatography. The chromatographic column was KromstarTM C18 (4.6 mm x 250 mm, 5 μm), mobile phase was acetonitrile (A)- 0.4% phosphoric acid aqueous solution (B), gradient elution, flow rate was 0.8 mL/min, column temperature was 25 ℃, the detection wavelength of sinapine thiocyanate, hyperoside, quercetin and kaempferol were 330, 354, 375, 363 nm, respectively, and the injection volume was 10 μL. With quercetin as the internal standard, the relative positive factors of quercetin and sinapine thiocyanate, Hyperoside and kaempferol were established, and the contents of four components were calculated to achieve multi-evaluation. At the same time, the contents of the four components were determined by external standard method, and the differences between calculated values and measured values were compared to verify the accuracy and feasibility of the method of quantitative analysis of multi-components by single marker. Results The average recoveries of sinapine thiocyanate, hyperoside, quercetin and kaempferol were 1.21%, 1.08%, 0.94% and 1.33%, respectively. The relative positive factors of quercetin and sinapine thiocyanate, hyperoside, kaempferol were 1.23%, 0.53% and 1.41%, respectively. There was no significant difference between the calculated and measured values of the four components in three batches of Shanhe lipid-lowering powder (P > 0.05). Conclusion It is accurate and feasible to determine the four components in Shanhe Jiangzhi Powder by quantitative analysis of multi-components by single marker, which has guiding significance for the quality control of Shanhe Jiangzhi Powder.