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[摘要]
目的 建立RP-HPLC法同时测定用于干预刀豆蛋白A(ConA)诱导的小鼠急性免疫性肝损伤的山茱萸萜类制剂(液体制剂)中莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸5种活性成分,为山茱萸萜类成分及其相关制剂的质量控制提供方法。方法 采用RP-HPLC法,Zorbax SB-C18柱(150 mm×4.6 mm,5 μm)色谱柱;以乙腈-添加2 mmol/L γ-环糊精的0.1%磷酸水溶液为流动相,梯度洗脱;体积流量1.0 mL/min;柱温30℃;检测波长240、360、210 nm;进样量3 μL。结果 莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸的线性范围分别为10.42~333.33、23.44~750.00、9.11~291.67、10.42~333.33、13.02~416.67 mg/L;供试样品中莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸的平均回收率为95.60%~98.02%,RSD为1.47%~1.89%;重复性试验RSD为1.46%~1.71%;稳定性试验RSD为1.29%~1.76%;6批山茱萸萜类制剂中含有莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸的平均质量浓度分别为669.6~680.2、850.1~869.5、94.1~96.4、164.3~166.1、85.6~87.6 mg/L。结论 该方法简便、灵敏度高、重复性好、回收率高,可用于检测山茱萸萜类制剂中莫诺苷、马钱苷、山茱萸新苷、齐墩果酸及熊果酸。
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[Abstract]
Objective To establish RP-HPLC strategy to simultaneously determine the terpenoids constitute of Corni Fructus preparation which is useful for the intervention of acute immunological liver injury in mice induced by concanavalin A (ConA), including morroniside, loganin, cornuside, oleanolic acid and ursolic, thus providing a scientific basis on the quality controls of Corni Fructus terpenoids and related medicinal preparations. Methods RP-HPLC method and Zorbax SB-C18 column (150 mm×4.6 mm, 5 μm) chromatographic column were employed; 2 mmol/L γ-cyclodextrin was added into the mobile phase containing acetonitrile and 0.1% ortho-phosphoric acid for gradient elution; The volume flow was 1.0 mL/min, the column temperature was 30℃ and the detection wavelengths were 240, 360, and 210 nm; The injection volume was 3 μL. Results The linear range in morroniside, loganin, cornuside, oleanolic acid, and ursolic acid was 10.42-333.33, 23.44-750.00, 9.11-291.67, 10.42-333.33, and 13.02-416.67 mg/L, respectively; The average recovery in the selected samples was 95.60%-98.02%, RSD was 1.47%-1.89%; The repeatability RSD was 1.46%-1.71%; The stability RSD was 1.29%-1.76%; Six batches of the Corni Fructus terpenoids medicinal preparation contained the average quality of morroniside, loganin, cornuside, oleanolic acid, and ursolic acid respectively was 669.6-680.2,850.1-869.5, 94.1-96.4, 164.3-166.1, and 85.6-87.6 mg/L. Conclusion The method established in this study is a credible way to determine the concents of morroniside, loganin, ornuside, oleanolic acid, and ursolic acid in the Corni Fructus terpenoids medicinal preparation with its simplicity, good repeatability, high sensibility and recovery rate.
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