心痛舒喷雾剂HPLC指纹图谱、含量测定及指标成分传递规律研究

HPLC fingerprint,content determination and transferring patterns of index components of Xintongshu spray

目的建立心痛舒喷雾剂高效液相色谱(HPLC)指纹图谱,对其指认成分进行含量测定,并探究饮片、中间体、喷雾剂中指标成分的传递规律,为心痛舒喷雾剂的工艺把关和质量控制提供参考。方法采用《中药色谱指纹图谱相似度评价系统(2012版)》建立13批心痛舒喷雾剂的HPLC指纹图谱,并指认共有峰;采用HPLC法对指认成分进行含量测定;以牡丹皮中的丹皮酚和川芎中的阿魏酸为指标成分,考察两者在饮片、中间体、喷雾剂中的传递规律。结果13批心痛舒喷雾剂中共有33个共有峰,相似度均≥0.994;共指认了8个成分,分别为没食子酸(5号峰)、氧化芍药苷(9号峰)、绿原酸(10号峰)、咖啡酸(14号峰)、芍药苷(17号峰)、阿魏酸(21号峰)、洋川芎内酯Ⅰ(27号峰)、丹皮酚(31号峰)。8个成分的含量分别为0.5903~0.7197、0.5657~0.8513、0.2794~0.3681、0.0806~0.1061、1.9225~3.0335、0.1513~0.1916、0.2506~0.3360、3.0567~4.1610 mg/mL。丹皮酚和阿魏酸从饮片→喷雾剂的平均转移率分别为63.76%、38.06%,其中在牡丹皮的渗漉提取和减压浓缩工艺中丹皮酚的损失超30%,在川芎的水蒸气蒸馏提取工艺中阿魏酸的损失超50%。结论建立的心痛舒喷雾剂HPLC指纹图谱及含量测定方法重复性好、专属性强;牡丹皮的渗漉提取和减压浓缩及川芎的水蒸气蒸馏提取是引起指标成分转移率下降的关键工艺。

OBJECTIVE To establish the HPLC fingerprint of Xintongshu spray,determine the contents of identified components,and investigate the transferring patterns of the index components of decoction pieces,intermediates and spray,so as to provide scientific reference for technology management and quality control of Xintongshu spray.METHODS HPLC fingerprints of 13 batches of Xintongshu spray were established by the Similarity Evaluation System for Chromatographic Fingerprints of TCM(2012 edition),and common peaks were identified;the contents of identified components were determined by HPLC.The paeonol in Moutan Cortex and ferulic acid in Chuanxiong Rhizoma were used as index components to investigate the transferring patterns of them in decoction pieces,intermediates and spray.RESULTS There were a total of 33 common peaks in the fingerprints of 13 batches of Xintongshu spray,and the similarities were more than 0.994.Eight components were identified,i.e.gallic acid(peak 5),oxypaeoniflorin(peak 9),chlorogenic acid(peak 10),caffeic acid(peak 14),paeoniflorin(peak 17),ferulic acid(peak 21),senkyunolideⅠ(peak 27)and paeonol(peak 31).The contents of 8 components ranged from 0.5903-0.7197,0.5657-0.8513,0.2794-0.3681,0.0806-0.1061,1.9225-3.0335,0.1513-0.1916,0.2506-0.3360,3.0567-4.1610 mg/mL,respectively.The average transfer rates of paeonol and ferulic acid from decoction pieces to sprays were 63.76%and 38.06%,respectively.It was also found that the process in which the loss of paeonol was more than 30%was the extraction by percolation and negative pressure concentration of Moutan Cortex.The process in which the loss of ferulic acid was more than 50%was the steam distillation extraction process of Chuanxiong Rhizoma.CONCLUSIONS The established HPLC fingerprint and content determination method of Xintongshu spray are reproducible and specific.The key processes that cause a decrease in the average transfer rates of the index components are the extraction by percolation and negative pressure concentration of Moutan Cortex and steam distillation extraction of Chuanxiong Rhizoma.