细辛标准煮散剂的质量评价

Quality Evaluation of Standard Decoction Prepared from Powder of Asari Radix et Rhizoma

目的:研究和建立细辛标准煮散剂的质量控制。方法:用中药饮片标准煮散剂的制备方法得到不同产地细辛饮片的标准煮散剂;运用高效液相色谱法,计算不同规格细辛煮散剂中细辛脂素的含量、出膏率、转移率等参数,建立指纹图谱,并通过方法学进行验证,对细辛饮片标准煮散剂进行质量评价。采用超高效液相色谱-四极杆飞行时间串联质谱法(UPLC-QTOF-MS)对主要色谱峰进行结构确认,明确细辛标准煮散剂的主要化学成分。结果:细辛脂素在线性范围内表现出良好的线性关系,方法学验证其稳定性、精密度、重复性试验的相对标准偏差(RSD)均<3.0%。转移率范围9.25%~11.0%,出膏率范围25.76~28.25 mg/mL,细辛饮片标准煮散剂的指纹图谱相似度>90.0%。采用液质分析,共鉴定出了16种化学成分。细辛中仅含的马兜铃酸类成分是马兜铃酸I、马兜铃酸D和马兜铃内酰胺I。结论:建立了细辛标准煮散剂的质量评价方法。

Objective:To establish the method for the quality control of the standard decoctions prepared from the powder of Asari Radix et Rhizoma.Methods:According to the preparation method of standard decoctions of Chinese medicinal material powder,the decoctions were prepared from the powder of Asari Radix et Rhizoma samples produced in different areas.High performance liquid chromatography(HPLC)was employed to determine the content,yield,and transfer rate of asarinin in the decoctions,and the HPLC fingerprint was established.Furthermore,the main components in the decoctions were identified by ultra-performance liquid chromatography-quadrupole time of flight-mass spectrometry(UPLC-QTOF-MS)for the main peaks.Results:Asarinin showed a good linear relationship within the tested concentration range.The methodological investigation showed that the relative standard deviations of the stability,precision,and repeatability were all less than 3%.The transfer rate ranged from 9.25%to 11.0%,and the yield from 25.76 mg/mL to 28.25 mg/mL.The fingerprint similarity of the decoctions prepared from the powder of Asari Radix et Rhizoma was greater than 90.0%.A total of 16 compounds were identified,including aristolochic acid I,aristolochic acid D,and aristolactam I.Conclusion:The quality evaluation method for the standard decoctions prepared from the powder of Asari Radix et Rhizoma was established.