小儿解表颗粒指纹图谱的建立及化学成分分析

Fingerprint and chemical composition analysis for Xiaoer Jiebiao Granule

目的:建立小儿解表颗粒的超高效液相色谱串联四极杆飞行时间质谱(UPLC-QTOF MS)指纹图谱,确认其化学成分并同时测定17个指标性物质的含量,结合聚类分析技术,对其进行系统、科学地质量评价。方法:采用UPLC-QTOF MS法对不同厂家的小儿解表颗粒进行分析,绘制10批样品的指纹图谱,运用中药色谱指纹图谱相似度软件进行相似度评价,并通过SPSS 23.0软件进行聚类分析;采用提取离子色谱测定17种化学成分的含量。结果:10批样品共确定28个共有峰,相似度均大于0.98,样品共聚为2类,指认了17种成分,这些成分的定量分析方法具有良好的线性关系(R2>0.9991)、极低的检出限(0.02~0.94μg·mL-1)、精密度和重现性较好(RSD<2%)、加标回收率在97.81%~102.48%(RSD<2.88%)。结论:建立的UPLC-QTOF MS方法准确实用,可用于小儿解表颗粒的质量评价。

OBJECTIVE Establishing an ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry(UPLC-QTOF MS)fingerprint analysis method combined with clustering analysis technique to confirmed the main composition as well the content of 17 substances of Xiaoer Jiebiao Granule for systematic and scientific quality evaluation.METHODS UPLC-QTOF MS was used to analyze Xiaoer Jiebiao Granule from different manufacturers to obtain the fingerprint of 10 batches of samples.The similarity of fingerprint was evaluated bysimilarity evaluation system of traditional Chinese medicine chromatographic fingerprints.Cluster analysis was performed by SPSS 23.0software.The contents of 17 chemical components were determined using extracted ion chromatography.RESULTS 28 common peaks in 10 batches were identified with similarity greater than0.98.The cluster analysis could group 10 batches of Xiaoer Jiebiao Granule into two categories,and 17 chemical components were confirmed.The quantitative analysis method had a good linear relationship(R2>0.9991),very low detection limit(0.02-0.94μg·mL-1),good precision and reproducibility(RSD<2%).The recovery rate was between 97.81%-102.48%(RSD<2.88%).CONCLUSION The established UPLC-QTOF MS method is accurate and practical,can be used to evaluate the quality of Xiaoer Jiebiao Granule.