目的:建立HPLC 波长切换法同时测定首荟通便胶囊中2,3,5,4'- 四羟基二苯乙烯-2-O-β-D-葡萄糖苷、柚皮苷、新橙皮苷和芦荟苷4 个活性成分的含量。方法:采用Kromasil C18 色谱柱(4.6 mm ×250mm,5 μm),以乙腈为流动相A 和0.1% 磷酸水溶液为流动相B,梯度洗脱,流速1.0 mL·min-1,柱温30 ℃,检测波长320 nm(0~25 min 时,检测2,3,5,4'- 四羟基二苯乙烯-2-O-β-D- 葡萄糖苷)、283 nm(25~38min 时,检测柚皮苷和新橙皮苷)、355 nm(38~60 min 时,检测芦荟苷)。结果:2,3,5,4'- 四羟基二苯乙烯-2-O-β-D- 葡萄糖苷、柚皮苷、新橙皮苷和芦荟苷的进样量分别在0.049 88~0.249 4 μg(r=0.999 9)、0.100 1~0.500 6 μg(r=0.999 8)、0.071 22~0.356 1 μg(r=0.999 9)、0.360 4~1.801 8 μg(r=0.999 7)范围内与峰面积呈良好线性关系;加样回收率(n=6)分别为98.9%,99.2%,99.0% 和98.9%,RSD 均小于1.0%。10批供试样品中,上述2,3,5,4'- 四羟基二苯乙烯-2-O-β-D- 葡萄糖苷等4 个成分的含量测定结果(n=6)依次为6.312~7.896、16.238~18.532、10.602~12.316 和60.289~66.731 mg·g-1。结论:建立的HPLC 波长切换法可同时测定首荟通便胶囊中4 个活性成分,且方法简便、快速、准确,可用于首荟通便胶囊的质量控制。
Objective: To establish an HPLC wavelength switching method for simultaneous determination of the contents of 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside,naringin,neohesperidin and aloin in Shouhui Tongbian capsules. Methods: The chromatographic separation was performed on Kromasil C18 column (4.6 mm×250 mm,5 μm),and gradient elution was conducted with acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B.The flow rate was 1.0 mL·min-1,and the column temperature was set at 30 ℃.The detection wavelength was chosen at 320 nm for 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside during 0-25 min,283 nm for naringin and neohesperidin during 25-38 min,and 355 nm for aloin during 38- 60 min. Results: The linear ranges of 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside,naringin, neohesperidin and aloin were 0.049 88-0.249 4 μg(r=0.999 9),0.100 1-0.500 6 μg(r=0.999 8),0.071 22-0.356 1 μg(r=0.999 9)and 0.360 4-1.801 8 μg(r=0.999 7),respectively.The average recoveries(n=6) were 98.9%, 99.2%,99.0% and 98.9%,respectively,with RSDs less than 1.0%.The content ranges of ten batches of samples were 6.312-7.896,16.238-18.532,10.602-12.316 and 60.289-66.731 mg·g-1,respectively. Conclusion: The HPLC wavelength switching method has been established for simultaneous determination of the contents of four active components in Shouhui Tongbian capsules.The method is simple,rapid and accurate,which can be used for the quality control of Shouhui Tongbian capsules.
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