[关键词]
[摘要]
目的 借助UPLC定量指纹图谱与UPLC-QE-Plus-MS/MS技术,研究吴茱萸Euodiae Fructus[石虎Euodia rutaecarpa (Juss.) Benth. var. officinalis (Dode) Huang]标准汤剂的量值传递规律。方法 通过对18批吴茱萸(石虎)样品进行检测,获得吴茱萸(石虎)饮片和标准汤剂的对照指纹图谱,并采用UPLC-QE-Plus-MS/MS技术,对标定的吴茱萸(石虎)共有峰进行鉴定。通过峰个数传递、相似度比较、有效成分含量转移率、出膏率测定等,对吴茱萸(石虎)标准汤剂的量值传递规律进行研究。结果 在饮片与标准汤剂中共标定25个对照指纹图谱共有峰,包括5个生物碱类化合物(去氢吴茱萸碱、evodiaxinine、吴茱萸酰胺、吴茱萸碱、吴茱萸次碱)、12个有机酸类化合物(咖啡酰葡萄糖酸及其同分异构体、阿魏酰葡萄糖酸及其同分异构体、绿原酸、新绿原酸、隐绿原酸、阿魏酰奎宁酸等)、7个黄酮类化合物(香树素-7-O-β-D-葡萄糖苷、芦丁、金丝桃苷、柠檬黄素-3-O-芸香糖苷、柯伊利素-7-O-芸香糖苷、水仙苷、异鼠李素-3-O-β-D-葡萄糖苷)、1个柠檬苦素类化合物(柠檬苦素)。经测定饮片中25个共有峰均传递到标准汤剂中,共有峰传递率为100%。以每批次吴茱萸(石虎)饮片的指纹图谱为对照,对应批次标准汤剂的指纹图谱相似度均大于0.9。以有效成分柠檬苦素、吴茱萸碱、吴茱萸次碱为指标,吴茱萸(石虎)标准汤剂中指标成分的转移率均在其均值±30%范围内。18批标准汤剂的出膏率也在其均值±30%范围内。结论 制备过程量值传递情况稳定,制备工艺可行,可为吴茱萸(石虎)配方颗粒的质量标准研究提供依据。
[Key word]
[Abstract]
Objective To study the quantity value transfer of Wuzhuyu (Shihu) [Euodiae Fructus (Euodia rutaecarpa (Juss.) Benth. var. officinalis (Dode) Huang), EF(ERO)] standard decoction based on UPLC quantitative fingerprint and UPLC-QE-Plus-MS/MS technology. Methods The control fingerprints of EF(ERO) decoction pieces and standard decoction were obtained through the detection of 18 batches of samples. In addition, the common components in control fingerprints were identified by UPLC-QE-Plus-MS/MS technology. Subsequently, the quantity value transfer of EF(ERO) standard decoction was studied by analyzing the number of peaks, similarity comparison, effective ingredient transfer rate, and extract determination. Results A total of 25 common peaks were identified in the control fingerprints of decoction piece and standard decoction, which contain five alkaloid compounds (dehydroevodiamine, evodiaxinine, benzamide, evodiamine, rutecarpine), 12 organic acid compounds (caffeioyl gluconic acid and its isomers, feruloyl gluconic acid and its isomers, neochlorogenic, cryptochlorogenic acid, chlorogenic acid, feruloylquinic acid), seven flavonoid compounds (diosmetin-7-O-β-D-glucopyranoside, rutin, hyperoside, limocitrin-3-O-rutinoside, coriolis-7-O-rutinoside, narcissoside, isorhamnetin 3-O-β-D-glucoside), and one limonin compound (limonin). All the 25 common peaks in the decoction pieces were transferred to the standard decoction, and the peak transfer rate was 100%. Meanwhile, with each bath of EF(ERO) decoction piece’s fingerprint as the control, the similarity of the fingerprint of corresponding batch standard decoction were all greater than 0.9. Furthermore, the transfer rate of index components in standard decoction of EF(ERO) were determined by using active components limonin, evodiamine and rutaecarpine as indexes. The results were all within ± 30% of the mean value. In addition, the determination of 18 batches of standard decoction average dry paste rate were also within ± 30% of the mean value. Conclusion The study results indicated that the quantity value transfer of standard decoction was stable during the preparation process, and the processing technology was feasible, which can lay a foundation for the preparation technology and quality standard research of the formulation granule of EF(ERO).
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[基金项目]
省产业链科技创新联合体协同攻关项目“赣食十味——陈皮(樟头红)的关键技术研究”(20224BBG72001);江西“樟帮”特色有毒中药附子临江片配方颗粒质量标准化研究(2022年赣江新区重大科技攻关项目,2022001);基于质量标志物的中药经典名方标准化示范性研究(2020年江西省双千计划)