整合指纹图谱与多成分含量测定的酸枣仁汤质量评价研究  

Quality evaluation of Suanzaoren Decoction by integrating fingerprint and quantitative analysis of multi-component

作　　者：李佳涵 王慧 刘佳星 杜晨晖 闫艳[1] LI Jia-han;WANG Hui;LIU Jia-xing;DU Chen-hui;YAN Yan(Modern Research Center for Traditional Chinese Medicine,Shanxi University,Taiyuan 030006,China;Institute of Pharmaceutical&Food Engineering,Shanxi University of Chinese Medicine,Taiyuan 030619,China)

机构地区：[1]山西大学中医药现代研究中心,山西太原030006 [2]山西中医药大学中药与食品工程学院,山西太原030619

出　　处：《中草药》2022年第15期4698-4708,共11页Chinese Traditional and Herbal Drugs

基　　金：山西省自然科学基金面上项目(20210302123237);山西省自然科学基金面上项目(20210302123470);山西省卫生健康委“十大晋药”项目(ZYCZL 2020007);山西中医药大学青年科学家培育项目(2021PY-QN-07);山西省科学技术厅-地产中药功效物质研究与利用山西省重点实验室项目(201605D111004)。

摘　　要：目的 利用HPLC-DAD-ELSD分析技术,建立酸枣仁汤指纹图谱结合多成分含量测定方法,为其质量控制提供参考。方法 采用Phenomenex C色谱柱(250 mm×4.6 mm,5.0μm),以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,体积流量为1.0 mL/min,柱温30℃,在282 nm和335 nm检测波长下,分别以芒果苷和斯皮诺素为参照峰;ELSD漂移管温度105℃,载气体积流量2.5 L/min条件下,以酸枣仁皂苷A为参照峰,采用中药色谱指纹图谱相似度评价系统对10批自制酸枣仁汤进行相似度评价;同时建立13个指标成分含量测定方法,应用于市售产品及自制样品的质量评价。结果 10批自制酸枣仁汤的平均出膏率为21.57%,在282 nm和335 nm分别标定了5个和4个共有峰,相似度分别为0.907~0.999、0.926~0.999;HPLC-ELSD指纹图谱中标定了4个共有峰,相似度为0.946~0.999。13种指标成分在各自的线性范围内线性关系良好(r>0.995 9),平均加样回收率为93.69%,RSD值平均为2.04%。10批不同剂型市售产品中新芒果苷、乌药碱、芒果苷、异芒果苷、甘草苷、斯皮诺素、阿魏酸、6′′′-阿魏酰斯皮诺素、异甘草苷、知母皂苷BII、酸枣仁皂苷A、酸枣仁皂苷B和甘草酸的质量分数分别为0.30~3.38、0.02~0.20、0.27~6.04、0.33~1.38、1.54~12.02、0.16~0.87、0.16~1.27、0.04~0.35、0.25~3.12、3.66~20.92、0.36~0.98、0.32~0.89、4.90~36.37 mg/g,波动范围大。自制酸枣仁汤13种成分含量波动范围小。结论 建立了酸枣仁汤HPLC-DAD-ELSD指纹图谱与多成分含量测定相结合的质量评价方法,方法准确、可靠,为市售酸枣仁汤产品的质量控制和体内药动学研究提供参考。Objective To develop the HPLC fingerprint combined with multi-component content determination method to comprehensively evaluate the quality of Suanzaoren Decoction(SZRD). Methods Chromatographic separation was operated at 30 ℃ on a Phenomenex C(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of 0.1% formic acid(A) and acetonitrile(B) for gradient elution, and the flow rate was set at 1.0 mL/min. Mangiferin and spinosin were chosen as reference peaks under detection wavelength of 282 nm and 335 nm, respectively. The drift tube of ELSD was set at 105 ℃ with the nebulizing gas flow rate of 2.5L/min and jujuboside A as reference peak. Similarity evaluation system for chromatographic fingerprint of TCM was used to evaluate the similarity of 10 batches of SZRD, and a quantitative analysis method of SZRD was established by HPLC-DAD-ELSD and applied to determine 10 batches of SZRD and 10 batches of SZRD commercial products. Results The average yield of 10 batches of SZRD’s dry extract was 21.57%. Five and four common peaks were calibrated in HPLC-DAD fingerprint at 282 nm and 335 nm, with their similarity ranged from 0.907 to 0.999, from 0.926 to 0.999, respectively. Four common peaks were calibrated in HPLC-ELSD fingerprint, and the similarity ranged from 0.946 to 0.999. All the calibration curves showed good linearity with correlation coefficients(r) no less than 0.9959, the average recovery was 93.69%, and the average RSD was 2.04%. The content of neomangiferin, coclaurine,mangiferin, isomangiferin, liquiritin, spinosin, ferulic acid, 6′′′-feruloylspinosin, isoliquiritin, timosaponin BII, jujuboside A, jujuboside B and glycyrrhizic acid in 10 SZRD commercial products in different dosage forms were 0.30—3.38, 0.02—0.20, 0.27—6.04, 0.33—1.38, 1.54—12.02, 0.16—0.87, 0.16—1.27, 0.04—0.35, 0.25—3.12, 3.66—20.92, 0.36—0.98, 0.32—0.89, 4.90—36.37 mg/g,respectively. Conclusion The results indicated that the new approach was applicable in the routine analysis and quality control of S

关 键 词：酸枣仁汤 高效液相色谱法 指纹图谱 多成分含量测定 质量评价 新芒果苷 乌药碱 芒果苷 异芒果苷 甘草苷 斯皮诺素 阿魏酸 6′′′-阿魏酰斯皮诺素 异甘草苷 知母皂苷BII 酸枣仁皂苷A 酸枣仁皂苷B 甘草酸 

分 类 号：R286.02[医药卫生—中药学]