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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。
OBJECTIVE: To elucidate the chemical constituents of the main tetracyclic terpenoids in melon pedicels and establish a HPLC method for the determination of cucurbitacin B and cucurbitacin D in melon pedicels. METHODS: The main tetracyclic triterpenes in melon stigma were analyzed by UPLC-ESI-Orbitrap-MS / MS. Eclipse XDB-C 18 column (4.6 mm × 150 mm, The mobile phase consisted of acetonitrile and acetonitrile. The contents of cucurbitacin B and cucurbitacin D in seven batches of melon leaves were determined by RP-HPLC. The chromatographic column (4.6 mm × 250 mm, 5 μm) on Inert Sustain C 18 column % Glacial acetic acid solution (containing 1 g · L ~ (-1) heptane sulfonate) -acetonitrile as the mobile phase at a detection wavelength of 228 nm. Results: In the qualitative analysis of chemical model, a total of eight major tetracyclic triterpene constituents in melon pedicle were identified and initially identified, including the genistein, isochrillin, cucurbitacin I, cucurbitacin D, B and deacetyl cucurbitacin B three isomers; quantitative analysis, cucurbitacin B, cucurbitacin D and related substances were satisfactory, the mass concentration of 49.5 ~ 297.0 mg The linear relationship was obtained between L -1 (r = 0.999 99) and 10.3 ~ 61.8 mg · L -1 (r = 0.999 9), with the average recoveries of 99.18% and RSD 1.0 %; 99.13%, RSD 1.1%. Conclusion: This study basically elucidated the main tetracyclic triterpenes in melon pedicle, and established a HPLC method for quantitative analysis with high accuracy and repeatability. It can be used in the cucurbitacin B cucurbitacin D content determination.