HPLC波长切换联合梯度洗脱法同时测定消疲灵颗粒中的7种成分

Simultaneous Determination of Seven Components in Xiaopiling Granule by HPLC Wavelength Switching Combined Gradient Elution Method

关键词:  消疲灵颗粒  牡荆素葡萄糖苷  牡荆素鼠李糖苷  牡荆素  金丝桃苷  芒柄花苷  毛蕊异黄酮  芒柄花素  波长切换联合梯度洗脱法  中成药多组分测定

Key words:  Xiaopiling granule  vitexin-4”-O-glucoside  vitexin-2”-O-rhamnoside  vitexin  hyperoside  ononin  calycosin  formononetin  wavelength switching combined gradient elution method  multicomponent determination of chinese patent drug

摘要:

目的 建立同时测定消疲灵颗粒中7种成分含量的HPLC波长切换联合梯度洗脱方法。方法 采用Venusil MP-C₁₈色谱柱，流动相为乙腈-1%冰醋酸溶液，流速为0.9 mL·min^-1，梯度洗脱，柱温为30 ℃，进样量为10 μL。结果 牡荆素葡萄糖苷、牡荆素鼠李糖苷、牡荆素、金丝桃苷、芒柄花苷、毛蕊异黄酮和芒柄花素检测浓度分别在2.56~51.20 μg·mL^-1，14.87~297.40 μg·mL^-1，2.14~42.80 μg·mL^-1，3.16~63.20 μg·mL^-1，3.80~76.00 μg·mL^-1，2.14~42.80 μg·mL^-1，4.81~ 96.20 μg·mL^-1内与峰面积呈良好的线性关系（r≥0.999 1），平均回收率97.0%~100.0%，RSD 0.55%~1.67%，精密度和重复性良好，供试品溶液在室温条件下12 h内稳定。结论 该方法操作简便，精密度、稳定性、重复性好，可用于消疲灵颗粒中7种有效成分含量的同时测定。

Abstract:

OBJECTIVE To develop an HPLC wavelength switching combined gradient elution method for determination of seven components in Xiaopiling granule simultaneously. METHODS The determination was performed on Venusil MP-C₁₈ column with mobile phase consisted of acetonitrile(A)-1% glacial acetic acid solution (B) at the flow rate of 0.9 mL·min^-1, gradient elution and the injection volum was 10 μL. The column temperature was 30 ℃. RESULTS The linear ranges of vitexin-4”-O-glucoside, vitexin-2”-o-rhamnoside, vitexin, hyperoside, ononin, calycosin and formononetin were 2.56- 51.20 μg·mL^-1, 14.87-297.40 μg·mL^-1, 2.14-42.80 μg·mL^-1, 3.16-63.20 μg·mL^-1, 3.80-76.00 μg·mL^-1, 2.14-42.80 μg·mL^-1, 4.81-96.20 μg·mL^-1, respectively(r≥0.999 1); the average recoveries were 97.0%-100.0% and the corresponding RSD was 0.55%-1.67%, respectively. The precision and the repeatability were good. Test solution was stable at room temperature in 12 h. CONCLUSION The method is simple with good precision, stability and reproducibility, and it can be used for the simultaneous determination of 7 components in Xiaopiling granule.