大黄标准汤剂量值传递规律研究

Study on law of quality value transmitting of Rhei Radix et Rhizoma standard decoction

目的研究大黄标准汤剂的量值传递规律。方法制备23批大黄标准汤剂,建立标准汤剂及其原料饮片的HPLC指纹图谱,标定共有峰,采用四级杆飞行时间高分辨质谱(quadrupole time-of-flight mass spectrometry,Q-TOF-MS/MS)对共有峰进行鉴定,分别测定饮片和标准汤剂中8个结合型蒽醌(芦荟大黄素-8-O-葡萄糖苷、大黄酸-8-O-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄酚-1-O-葡萄糖苷、大黄酚-8-O-葡萄糖苷、芦荟大黄素-3-羟甲基-O-葡萄糖苷、大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷)、5个游离型蒽醌(芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚)、4个鞣质类成分(没食子酸、儿茶素、表儿茶素、表儿茶素没食子酸酯)和1个二苯乙烯类成分[白藜芦醇4′-O-β-D-(6″-O-没食子酰)-葡萄糖苷(RGG)]的含量及标准汤剂出膏率,以共有峰传递数、成分转移率及出膏率为指标,分析大黄标准汤剂的量值传递规律。结果大黄饮片指纹图谱标定共有峰45个,其中40个传递到了标准汤剂,40个共有峰的成分均得到鉴定,其中8个结合型蒽醌、5个游离型蒽醌、2个蒽酮类成分、5个鞣质类成分、2个二苯乙烯类成分采用对照品比对确认。8个结合型蒽醌和5个游离型蒽醌合计的平均转移率分别为43.83%和11.03%,没食子酸、儿茶素、表儿茶素和表儿茶素没食子酸酯的平均转移率分别为233.00%、79.58%、303.18%和58.71%,RGG的平均转移率为68.89%,标准汤剂平均出膏率为23.26%。结论研究结果为大黄配方颗粒和含大黄经典名方制剂工艺研究和质量评价奠定了基础。

Objective To study the law of quality value transmitting of Dahuang(Rhei Radix et Rhizoma,RRR)standard decoction.Methods Twenty-three batches of RRR standard decoction were prepared.The HPLC fingerprints of standard decoction and decoction pieces were established.The common peaks in fingerprints were assigned and the components of common peaks were identified by Q-TOF-MS/MS.The contents of the components in raw pieces and standard decoctions of RRR were determined,including eight combination anthraquinones of aloe emodin-8-O-glucoside(AE8G),rhein-8-O-glucoside(R8G),emodin-1-Oglucoside(E1 G),chrysophanol-1-O-glucoside(C1 G),chrysophanol-8-O-glucoside(C8 G),aloe emodin-3-CH2-O-glucopyranoside(AE3 G),emodin-8-O-glucoside(E8 G)and physcion-8-O-glucoside(P8 G),five free anthraquinones of aloe emodin,rhein,emodin,chrysophanol and physcion,four tannins of gallic acid,catechin,epicatechin and epicatechin gallate,and one stilbene of resveratrol 4′-O-β-D-(6″-O-galloyl)-glucoside(RGG)in decoction pieces and standard decoction,and the extraction ratio of standard decoction were determined,respectively.Taking the transfer number of common peaks,component transfer rate and extraction ratio as indexes,the law of quality value transmitting of RRR standard decoction was analyzed.Results There were 45 common peaks in the fingerprint of RRR decoction pieces,40 of which were transferred to the standard decoction.The components of 40 common peaks were identified,among them,eight combination anthraquinones,five free anthraquinones,two anthrones,five tannins and two stilbenes were confirmed by reference substances.The average transfer rates of total eight combination anthraquinones and five free anthraquinones were 43.83%and 11.03%,and that of gallic acid,catechin,epicatechin,epicatechin gallate and RGG were 233.00%,79.58%,303.18%,58.71%and 68.89%,respectively.The average extraction rate of standard decoction was 23.26%.Conclusion The results of this study laid a foundation for the process research and quality evaluation of RRR dispensing granules and preparations of the classic prescriptions containing RRR.