Study On Quality Control Of Ganmaoling Granule

Ganmaoling granule is a preparation of Chinese and Western Medicine, belong to antipyretic analgesic drugs,which as a common cold medicine. Five Chinese traditioanal drugs: Wild chrysanthemum, Bidens biternata, Evodia lepta, Gang mei, Mint oil and three chemical medicine: acetyl paracetamol,caffeine,chlorphenamine maleate composition the Ganmaoling granule. Current drug standard of Ganmaoling granule is included in the Chinese traditional patent formulation,Twelfth volumes of Chinese herbal preparation, which test items mainly include the thin layer chromatography identification of acetaminophen and chlorphenamine maleate and titration method for the determination content of acetaminophen. The work of thin layer chromatography of prescription in three kinds of chemical drugs and Wild chrysanthemum ingredient identification was reported presently. HPLC method for the determination content of acetyl paracetamol, caffeine, chlorphenamine maleate and Wild chrysanthemum ingredients were reported, but it is difficult to control Ganmaoling granule quality overallly. This system research basis on the technology of UPLC-Q-TOF-MS and UPLC, aim to provide scientific theory for quality control of Ganmaoling granule.1. Identification of chemical components of Ganmaoling granule by UPLC-Q-TOF-MS.This study using ultra performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry(UPLC-Q- TOF-MS) technology for qualitative analysis of main chemical components of Ganmaoling granule. Using ACQUITY UPLC HSS C18(2.1 mm ×50 mm, 1.8 μm)chromatographic column, acetonitrile-0.1% formic acid solution as mobile phase in gradient elution,volume flow rate is 0.15 m L/min. The injection volume was 2 μL. The ESI ion source mass spectrometry are positive and negative ion mode scanning data acquisition. Through the positive and negative ion mass spectrometry and elemental composition analysis and then combined with the relevant literature and control data mode, this study identified 11 compound of Ganmaoling granule,they are: chlorogenic acid,neochlorogenic acid,chlorogenic acid,isochlorogenic acid A,isochlorogenic acid B,isochlorogenic acid C,muxi asiaticoside,mongolian linarin,acetyl paracetamol, caffeine and chlorphenamine maleate. This study provided a scientific basis for the mechanism and quality control of Ganmaoling granule.2. Study on ultra performance liquid chromatographic fingerprint of Ganmaoling granule.In this paper, an analytical method for the quality control of Ganmaoling granule by ultra performance liquid chromatography with high performance liquid chromatography was established. The samples were extracted with methanol by ultrasonic 30 min, and then 50% methanol was used to re dissolve, and the extraction liquid was analyzed by ultra performance liquid chromatography. Using ACQUITY UPLC HSS C18(2.1 mm ×50 mm, 1.8 μm)chromatographic column, acetonitrile-0.1% formic acid solution as mobile phase in gradient elution,volume flow rate is 0.15 m L/min, column temperature is 30℃. Results show that 22 common peaks at 30 min were separately, the similarity of 25 batches of samples reached 0.97,indicate a Ganmaoling granule product quality is stabilly. This method is fastly,efficiently and stably, morever, this method can be used for the quality control.3. Determination of seven kinds of component in Ganmaoling granule by UPLC.This study establish a method for determination content of seven kinds of component in Ganmaoling granule, they are: neochlorogenic acid, chlorogenic acid, luteolin, isochlorogenic acid C, linarin glycosides, caffeine and acetyl paracetamol. Using ACQUITY UPLC HSS C18( 2.1 mm ×50 mm, 1.8 μm) chromatographic column,acetonitrile-0.1% formic acid solution as mobile phase in gradient elution,volume flow rate is 0.15 m L/min.The detection wavelength was 264 nm and 310 nm, and the column temperature was 30℃. 7 component peak area and concentration has a good linear relationship, the average recovery rate was 98.9% ~ 100.9%, precision RSD is 1.67% ~ 4.69%. This method can be used for the quality control of Ganmaoling granule.