枳壳饮片标准汤剂质量评价研究

Study on Quality Evaluation of Aurantii Fructus Standard Decoction

目的建立枳壳标准汤剂的质量控制方法,为枳壳配方颗粒及其他枳壳产品的质量评价提供参考。方法按照标准汤剂制备要求,制备13批枳壳饮片标准汤剂,建立HPLC特征图谱。采用高效液相色谱串联四极杆飞行时间质谱(high performance liquid chromatography-quadrupole time-of-flight mass spectrometry,HPLC-Q-TOF-MS),电喷雾离子源,在正负离子模式下采集数据,对主要色谱峰进行定性鉴别。采用HPLC测定标准汤剂中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷4种成分含量,计算标准汤剂的出膏率、4种成分转移率和pH。结果HPLC特征图谱中共6个共有峰,通过质谱定性分析结合对照品比较,对6个共有峰进行了指认,分别为新北美圣草苷、芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷和枳属苷,13批枳壳饮片标准汤剂相似度均>0.98。枳壳标准汤剂中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷质量分数分别为0.07%~0.26%,1.30%~3.40%,0.14%~0.34%,0.85%~3.64%,转移率分别为31.4%~50.6%,31.3%~48.9%,22.9%~48.2%,25.3%~50.9%;出膏率为19.3%~30.71%;pH为3.45~4.64。结论建立的系统评价枳壳饮片标准汤剂的质量方法稳定可行,为枳壳标准汤剂及其相关制剂的质量评价提供科学依据。

OBJECTIVE To establish the quality control methods of Aurantii Fructus standard decoction and to provide reference for quality evaluation of Aurantii Fructus formula granules and other Aurantii Fructus products.METHODS According to the standard decoction preparation requirements,13 batches of Aurantii Fructus standard decoctions were prepared and HPLC fingerprint was established.The main chromatographic peaks were identified under the positive and negative ion mode by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(HPLC-Q-TOF-MS)and electrospray ionization source.The four chemical components(narirutin,naringin,hesperidin and neohesperidin)in the standard decoction were determined by HPLC.The extract rate,the transfer rate of the four flavonoid glycosides,and the pH of the standard decoction were calculated.RESULTS Six common peaks in the fingerprint were assigned by qualitative analysis of mass spectrometry and standard comparison,namely neoeriocitrin,narirutin,naringin,hesperidin,neohesperidin and poncirin.The fingerprint similarities of the 13 batches of standard decoctions were>0.98.The content ranges of narirutin,naringin,hesperidin and neohesperidin in the standard decoction were 0.07%-0.26%,1.30%-3.40%,0.14%-0.34%,0.85%-3.64%,respectively.The transfer rates of the four components were 31.4%-50.6%,31.3%-48.9%,22.9%-48.2%,25.3%-50.9%,respectively.The dry extract rates were 19.3%-30.71% and pH values were 3.45-4.64.CONCLUSION The established systematic evaluation method of the quality of the Aurantii Fructus standard decoction is stable and feasible and can provide a scientific basis for the quality evaluation of Aurantii Fructus standard decoction and related preparations.