甜瓜蒂中主要四环三萜结构鉴定及葫芦素B,葫芦素D含量测定

发布时间：2018-07-10 18:33

本文选题：甜瓜蒂 + 超高液相色谱-电喷雾-四级杆-静电场轨道质谱联用技术　；参考：《中国实验方剂学杂志》2017年08期

【摘要】：目的:阐明甜瓜蒂中主要四环三萜类成分化学模式,建立HPLC测定甜瓜蒂药材中葫芦素B和葫芦素D含量的方法。方法:采用UPLC-ESI-Orbitrap-MS/MS技术分析甜瓜蒂中主要的四环三萜类成分,Eclipse XDB-C_(18)色谱柱(4.6 mm×150 mm,5μm),以0.1%甲酸-乙腈溶液为流动相梯度洗脱;采用RP-HPLC法测定7批甜瓜蒂药材中葫芦素B和葫芦素D含量,Inert Sustain C_(18)色谱柱(4.6 mm×250 mm,5μm),以0.1%冰乙酸溶液(含庚烷磺酸钠1 g·L~(-1))-乙腈为流动相,检测波长228 nm。结果:在化学模式定性分析中,共发现并初步鉴定出甜瓜蒂中主要的8种四环三萜类成分,包括雪胆素甲,异雪胆素甲,葫芦素I,葫芦素D,葫芦素B及25-脱乙酰基葫芦素B的3个同分异构体;在定量分析中,葫芦素B,葫芦素D与有关物质分离度均符合要求,其质量浓度分别在49.5~297.0 mg·L~(-1)(r=0.999 99),10.3~61.8 mg·L~(-1)(r=0.999 9)与峰面积呈现良好的线性关系,平均回收率分别为99.18%,RSD 1.0%;99.13%,RSD 1.1%。结论:该研究基本阐明了甜瓜蒂中主要的四环三萜类成分,并建立了用于定量的HPLC方法,准确度高,重复性好,可用于甜瓜瓜蒂药材中葫芦素B,葫芦素D的含量测定。
[Abstract]:Objective: to elucidate the chemical pattern of main tetracyclic triterpenoids in sweet melon and to establish a HPLC method for the determination of cucurbitacin B and cucurbitacin D. Methods: UPLC-ESI-Orbitrap-MS / MS / MS technique was used to analyze the main tetracyclic triterpenoids in sweet melon pedicle with the column of 4.6 mm 脳 150mm ~ 5 渭 m), and mobile phase gradient elution of 0.1% formic acid-acetonitrile solution. A RP-HPLC method was used to determine the contents of cucurbitacin B and cucurbitacin D in 7 batches of sweet melon fruit. The column of Inert Sustain C _ (18) (4.6 mm 脳 250mm ~ 5 渭 m),) was used as mobile phase with 0.1% glacial acetic acid solution (containing 1 g / L ~ (-1) heptane sulfonate) -acetonitrile as the mobile phase, and the detection wavelength was 228 nm. Results: eight major tetracyclic triterpenoids were found and identified in the qualitative analysis of chemical models. Three isomers of Cucurbitacin I, Cucurbitacin D, Cucurbitacin B and 25-Deacetyl Cucurbitacin B. in quantitative analysis, the separation degree of Cucurbitacin B, Cucurbitacin D and related substances all meet the requirements. There was a good linear relationship between the peak area and the mass concentration of 49.5 ~ 297.0 mg / L ~ (-1) (r ~ (0.999) ~ (99) ~ (10. 3N) ~ (61.8) mg / L ~ (-1) (r ~ (0.999 9), respectively. The average recoveries were 99.18% (RSD = 1.0) and 99.13 ~ (13) RSD = 1.1, respectively. Conclusion: the main components of tetracyclic triterpenoids in sweet melon pedicle were elucidated in this study. A HPLC method was established for the determination of cucurbitacin B and cucurbitacin D in muskmelon melon pedicle with high accuracy and good reproducibility.
【作者单位】：北京市通州区食品药品安全监控中心;中国中医科学院中药研究所;
【基金】：中央本级重大增减支项目子课题(2060302)
【分类号】：R284.1;O657.72

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