分析测试学报2025，Vol.44Issue(5)：794-803,10.DOI:10.12452/j.fxcsxb.241114528
术通颗粒成分鉴定及多成分快速测定方法研究
Study on Identification and Rapid Determination of Multiple Compo-nents of Zhutong Granules
摘要
Abstract
Forty-nine components of Zhutong granules were identified based on ultra high perfor-mance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS/MS).Using high performance liquid chromatograph multi-wavelength detector(HPLC-MWD),a rapid determination method of 12 important chemical constituents in Zhutong granules was estab-lished with the aid of multiple dual wavelength switching.The Agilent Poroshell 120 EC-C18 chro-matographic column(4.6 mm×100 mm,2.7 μm)was used with 0.1%formic acid water-acetoni-trile as the mobile phase for gradient elution.The flow rate was set at 1.2 mL·min-1 with column tem-perature of 30℃and injection volume of 5 μL.Dual AJS ESI ion source quadrupole time-of-flight mass spectrometry was used to collect accurate molecular weight and fragment ion in positive and neg-ative ion modes.Through the establishment of Zhutong granules component database,49 major chemical components were screened and identified by accurate molecular weight matching,fragment ion and reference substance comparison.Dual wavelength switching(0-2 min,17-21 min,23-25 min,220 nm;2-17 min,21-23 min,283 nm)were used to determine 12 main components in Zhutong granules quantitatively within 25 min.Twelve major components reached baseline separation in dual-wavelength switching chromatograms with quantitation limits of 0.050 0-0.655 0 μg·mL-1.and recoveries of 98.3%-103%.The average contents of 12 components in 3 batches of Zhutong gran-ules were 0.060-16.597 mg·g-1.This method can rapidly determine more components with good sen-sitivity and accuracy,which is useful for quality control and subsequent new drug development of Zhutong granules.关键词
术通颗粒/成分鉴定/多成分测定/双波长切换Key words
Zhutong granules/chemical identification/multiple component quantitative analysis/dual wavelength switching分类
化学引用本文复制引用
陈奎,黄蓓蓓,刘洁,王腾腾,乔韵,蔡胜楠,石丽霞,李月婷,肖红斌..术通颗粒成分鉴定及多成分快速测定方法研究[J].分析测试学报,2025,44(5):794-803,10.基金项目
国家自然科学基金面上项目(82173957) （82173957）
国家自然科学基金青年基金项目(82204599) （82204599）
国家中医药管理局高水平中医药重点学科(中药分析学)建设项目(zyyzdxk-2023265) （中药分析学）
