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目的建立HPLC波长切换联合梯度洗脱法(HPLC-DVD法)同时测定越鞠片中9种指标成分α-香附酮、京尼平龙胆二糖苷、栀子苷、西红花苷I、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯和苍术素的量。方法采用HPLC-DVD法,Zorbax Eclipse Plus C_(18)(250 mm×4.6 mm,5μm)色谱柱;甲醇-乙腈(2∶1,A)-0.2%冰醋酸溶液(B)为流动相,进行梯度洗脱,体积流量0.9 m L/min;α-香附酮、京尼平龙胆二糖苷和栀子苷的检测波长为240 nm,西红花苷I的检测波长为440 nm,洋川芎内酯H、洋川芎内酯I、洋川芎内酯A和藁本内酯的检测波长为280 nm,苍术素的检测波长为340 nm;进样量为10μL。结果 9种指标成分α-香附酮在2.58~51.60μg/m L(r=0.999 4)、京尼平龙胆二糖苷在11.99~239.80μg/m L(r=0.999 9)、栀子苷在17.96~359.20μg/m L(r=0.999 6)、西红花苷I在3.98~79.60μg/m L(r=0.999 7)、洋川芎内酯H在2.82~56.40μg/m L(r=0.999 9)、洋川芎内酯I在2.38~47.60μg/m L(r=0.999 9)、洋川芎内酯A在6.04~120.80μg/m L(r=0.999 5)、藁本内酯在7.98~159.60μg/m L(r=0.999 3)、苍术素在6.51~130.20μg/m L(r=0.999 2)质量浓度与峰面积具有较好的线性关系;精密度良好,RSD≤1.22%;重复性良好,RSD≤1.75%;供试品溶液在室温条件下_(18) h内稳定,RSD≤1.37%;平均加样回收率和相应的RSD分别为97.64%(0.98%)、99.09%(1.46%)、100.11%(1.03%)、97.87%(0.80%)、98.59%(1.19%)、96.89%(1.34%)、99.38%(0.58%)、98.50%(1.22%)、99.71%(0.85%)。10批次供试品中α-香附酮、京尼平龙胆二糖苷、栀子苷、西红花苷I、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯和苍术素量分别为0.282~0.344、2.099~2.445、3.628~4.225、0.758~0.913、0.241~0.286、0.217~0.266、1.077~1.291、1.386~1.623、1.137~1.434mg/片。结论建立的HPLC-DVD法同时测定越鞠片中的9种成分,方法操作简便、快速、准确,可为越鞠片质量控制提供科学依据。
OBJECTIVE To establish HPLC-wavelength-switched combined gradient elution (HPLC-DVD method) for the simultaneous determination of nine indicator components, namely α-ketones, genipin, gentioside, crocin I, Yang Chuanxiong lactone H, Yang Chuanxiong lactone I, Yang Chuanxiong lactone A, ligustilide and the amount of atractate. Methods The HPLC-DVD method was used with a mobile phase of Zorbax Eclipse Plus C 18 (250 mm × 4.6 mm, 5 μm) and methanol-acetonitrile (2:1, A) -0.2% glacial acetic acid (B) Gradient elution, the volume flow rate of 0.9 m L / min; α-ketoconazole, genipin and geniposide detection wavelength of 240 nm, crocin I detection wavelength of 440 nm, Yang Chuanxiong Lactone H, Yang Chuanxiong lactone I, Yang Chuanxiong lactone A and ligustilide detection wavelength of 280 nm, the detection wavelength of atractylodes was 340 nm; injection volume of 10 μL. Results The results showed that the contents of α-ketoconazole in 9 kinds of indicators were between 2.58 ~ 51.60 μg / m L (r = 0.999 4), Genipin gentiobioside 11.99 ~ 239.80 μg / m L (r = 0.999 9) In the range of 17.96 ~ 359.20μg / m L (r = 0.999 6), crocin I was 3.98 ~ 79.60μg / m L (r = 0.999 7) = 0.999 9). The results showed that in the range of 2.38 ~ 47.60μg / m L (r = 0.999 9) and the ratio of the yangchuo xiong lactone A was 6.04-120.80μg / m L (r = 0.999 5) 7.98 ~ 159.60μg / m L (r = 0.999 3). The concentration of atractylitin in the range of 6.51 ~ 130.20μg / m L (r = 0.999 2) has a good linear relationship with the peak area; the precision is good with RSD≤1.22% ; Reproducibility was good with RSD≤1.75%. The sample solution was stable within 18 h at room temperature, RSD≤1.37%. The average recovery rate and the corresponding RSD were 97.64% (0.98%), 99.09 (1.46%), 100.11% (1.03%), 97.87% (0.80%), 98.59% (1.19%), 96.89% (1.34%), 99.38% (0.58%), 98.50% (0.85%). 10 batches of the test for alpha-ketones, genipin gentiobioside, geniposide, crocin I, Yang Chuanxiong lactone H, Yang Chuanxiong lactone I, Yang Chuanxiong lactone A, 藁The lactones and the total amount of herb were 0.282 ~ 0.344, 2.099 ~ 2.445, 3.628 ~ 4.225, 0.758 ~ 0.913, 0.241 ~ 0.286, 0.217 ~ 0.266, 1.077 ~ 1.291, 1.386 ~ 1.623 and 1.137 ~ 1.434mg / Conclusion The HPLC-DVD method was used to determine the contents of nine components in the Juju tablet at the same time. The method is simple, rapid and accurate, which can provide a scientific basis for the quality control of Juju tablets.