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目的建立HPLC-DAD波长切换联合梯度洗脱法同时测定博尔宁胶囊中12种指标成分毛蕊异黄酮葡萄糖苷、澳洲茄碱、澳洲茄边碱、重楼皂苷VII、重楼皂苷VI、重楼皂苷II、重楼皂苷I、特女贞苷、迷迭香酸、大黄酸、大黄酚和大黄素的量。方法采用HPLC-DAD法,Atlantis T3 C_(18)(250 mm×4.6 mm,5μm)色谱柱;乙腈-甲醇-0.1%甲酸水溶液为流动相,体积流量0.8 m L/min,梯度洗脱;变波长扫描;进样量为20μL。结果 12种指标成分毛蕊异黄酮葡萄糖苷、澳洲茄碱、澳洲茄边碱、重楼皂苷VII、重楼皂苷VI、重楼皂苷II、重楼皂苷I、特女贞苷、迷迭香酸、大黄酸、大黄酚和大黄素分别在1.97~19.70μg/m L(r=0.999 2)、1.022~10.220μg/m L(r=0.999 3)、0.982~9.820μg/m L(r=0.999 1)、1.1~11.0μg/m L(r=0.999 6)、1.154~11.540μg/m L(r=0.999 8)、1.114~11.140μg/m L(r=0.999 5)、1.102~11.020μg/m L(r=0.999 3)、2.768~27.680μg/m L(r=0.999 3)、3.04~30.40μg/m L(r=0.999 6)、3.379~33.790μg/m L(r=0.999 5)、3.286~32.860μg/m L(r=0.999 4)、3.507~35.070μg/m L(r=0.999 7)质量浓度与峰面积具有较好的线性关系;精密度、重复性良好,RSD均小于2.0%;平均加样回收率和相应的RSD分别为100.08%、1.27%;98.11%、1.15%;99.68%、1.13%;101.38%、0.87%;101.87%、0.95%;100.53%、0.74%;98.52%、0.83%;99.52%、0.88%;97.84%、1.33%;98.31%、0.71%;99.66%、0.57%;101.73%、1.41%。12批次供试品中12种指标成分质量分数分别为0.085~0.1_(18) mg/g、0.065~0.085 mg/g、0.051~0.075 mg/g、1.822~1.888 mg/g、1.532~1.599 mg/g、1.027~1.148 mg/g、2.420~2.621 mg/g、6.428~6.937 mg/g、0.258~0.289 mg/g、0.122~0.143mg/g、0.159~0._(18)4 mg/g、0.222~0.273 mg/g。结论建立的HPLC-DAD波长切换联合梯度洗脱法同时测定博尔宁胶囊中的12种成分,方法操作简便、快速、准确,可作为博尔宁胶囊全面可靠的质量控制方法。
OBJECTIVE To establish a HPLC-DAD coupled with wavelength-selective gradient elution method for the simultaneous determination of 12 indicators of berlin isoflavone glucoside, avermectin, nectarine, resplenoside VII, resplendent saponin VI, II, resplendent I, Chastain, rosmarinic acid, rhein, chrysophanol and emodin. Methods The HPLC-DAD method was used on a Atlantis T3 C18 (250 mm × 4.6 mm, 5 μm) column. The mobile phase was acetonitrile-methanol-0.1% formic acid solution and the volume flow rate was 0.8 m L / min. Wavelength scanning; injection volume of 20μL. Results 12 kinds of index components calycosin glucoside, avermectin, nectarine Australia, Tremella saponin VII, Tremella saponin VI, Tremella saponin II, Tremella saponin I, special virginia glycosides, rosmarinic acid, rhubarb The contents of acid, chrysophanol and emodin were in the range of 1.97-19.19μg / mL (r = 0.999 2), 1.022-10.220μg / mL (r = 0.999 3), 0.982-9.820μg / mL , 1.1 ~ 11.0μg / m L (r = 0.999 6), 1.154 ~ 11.540μg / m L (r = 0.999 8), 1.114-11.140μg / m L (r = 0.999 5), 1.102 ~ 11.020μg / m L (r = 0.999 3), 2.768-27.680 μg / m L (r = 0.999 3), 3.04-30.30 μg / m L (r = 0.999 6), 3.379-33.790 μg / m L ~ 32.860μg / m L (r = 0.999 4) and 3.507 ~ 35.070μg / m L (r = 0.999 7). The precision and repeatability of the results were good with RSD less than 2.0% ; The average recovery and corresponding RSD were 100.08%, 1.27%, 98.11%, 1.15%, 99.68%, 1.13%, 101.38%, 0.87%, 101.87%, 0.95%, 100.53%, 0.74%, 98.52% , 0.83%, 99.52%, 0.88%, 97.84%, 1.33%, 98.31%, 0.71%, 99.66%, 0.57%, 101.73%, 1.41%. The quality indexes of 12 indexes in 12 lots were 0.085-0.118 mg / g, 0.065-0.085 mg / g, 0.051-0.075 mg / g, 1.822-1.888 mg / g, 1.532-1.599 mg / g, 1.027 to 1.148 mg / g, 2.420 to 2.621 mg / g, 6.428 to 6.937 mg / g, 0.258 to 0.289 mg / g, 0.122 to 0.143 mg / g and 0.159 to 0.18 mg / g, 0.222 ~ 0.273 mg / g. Conclusion The established HPLC-DAD wavelength shift combined with gradient elution method for simultaneous determination of 12 components in Bortin capsule is simple, rapid and accurate and can be used as a comprehensive and reliable quality control method for Bolin capsule.