Basic Research On The Material Of Yinqin Capsule Based On Liquid Chromatography-mass Spectrometry

Objective:To establish the high performance liquid chromatogram of Yinqin Capsule,and preliminary identified its chemical composition by liquid chromatography-mass spectrometry,which provided an important basis for the quality consistency control of Yinqin Capsule.Methods:(1)By examining the total peak number and total peak area of the chromatographic peak,the extraction methods were screened from four aspects:solvent extraction,extraction time,content and extraction times,and the conditions for extracting Yinqin capsule were optimized.(2)By analyze the peak shape,baseline,resolution,retention time and other comprehensive indicators of high-performance liquid chromatography peaks of Yinqin Capsule,high performance liquid chromatography(HPLC)from five aspects:detection wavelength,mobile phase selection,gradient conditions,flow rate and column temperature The method was optimally selected,and the experimental data were compared to determine the optimal experimental method for the HPLC separation of Yinqin Capsule.(3)Based on the high-performance liquid phase separation method of Yinqin Capsule,the chemical constituents of the materials in Yinqin Capsules were analyzed by LC-MS,and the peaks were determined for some of the peaks.Results:(1)Considering the analysis results of various factors,the method of ultrasonic extraction of Yinqin Capsule is methanol as extraction solvent,the extraction time is 30 min,the content is 0.48 g,and the extraction times are 2 times.(2)High-performance liquid chromatography conditions of Yinqin Capsule were established,that is,X Bridge C18(4.6mm×250mm,5μm)column,acetonitrile(A)-0.1%(v/v)formic acid aqueous solution(B)was used as mobile phase:0-2 min,5%A-5%A;2-5 min,5%A-10%A;5-10 min,10%A-20%A;10-20 min,20%A-20%A;20-30 min,20%A-30%A;30-60 min,30%A-55%A;60-65 min,55%A-55%A,65-66min,55%A-5%A;66-70min,5%A-5%Agradient elution,detection wavelength:280 nm;flow rate:1.0 mL/min;injection amount:10μL,column temperature 25℃.(3)The analytical conditions of the liquid chromatography-mass spectrometry of Yinqin Capsule were established.The material basis of the Yinqin Capsule extract was studied by ESI positive and negative ion mode,Full MS-SIM mode,scanning range:m/z 150-2000 and other mass spectrometry parameters to study the material basis of Yinqin Capsule extract.By comparing the sample with the reference ion peak and consulting the relevant references,a total of 32 compounds and their peak assignments were determined in the extract of Yinqin Capsule.Conclusions:(1)The optimal ultrasonic extraction conditions for the extraction of Yinqin Capsules were determined.(2)A high performance liquid chromatography method was developed for the separation of chemical constituents from the extract of Yinqin Capsule.(3)The experimental method of liquid-mass spectrometry was established.The material of the silver carp capsule extract was studied.The compound components of 32 chromatographic peaks were estimated,and the chromatographic peaks were determined.