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Article in Chinese | WPRIM | ID: wpr-828018


UHPLC-LTQ-Orbitrap-MS was developed for the identification of chemical constituents in Qingfei Paidu Decoction, which will clarify its material basis. ACQUITY UHPLC HSS T3 chromatography column(2.1 mm×100 mm, 1.8 μm) was used with 0.1% formic acid(B)-acetonitrile(A) as the mobile phase in gradient elution. The decoction was detected by high-resolution liquid chromatography-mass spectrometry equipped with an ESI ion source in positive and negative mode. Based on the accurate mass measurements, retention time, mass fragmentation patterns combined with comparison of reference and literature reports, a total of 87 major compounds including 43 flavonoids, 9 alkaloids, 4 triterpenoid saponins, 1 sesquiterpene, 2 coumarins, 10 phenolic acids and 18 other compounds were tentatively screened and characterized. UHPLC-LTQ-Orbitrap-MS was employed to comprehensively elucidate the chemical components in Qingfei Paidu Decoction, which basically covered 20 Chinese medicines except gypsum in Qingfei Paidu Decoction. These collective results provide a scientific basis for further research on the quality control standard of Qingfei Paidu Decoction.

Chromatography, High Pressure Liquid , Coumarins , Drugs, Chinese Herbal , Flavonoids , Mass Spectrometry
Article in Chinese | WPRIM | ID: wpr-801945


Objective: To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ MS) method for the simultaneous determination of twelve components (wogonoside,baicalin,wogonin,chrysin,uteolin,caffeic acid,acetylcorynoline,corynoline,protopine,salicylic acid,uracil and adenosine) in Pudilan Xiaoyan oral liquid. Method: The analysis was performed on an Agilent Extend C18 column(3.0 mm×150 mm,3.5 μm),with a gradient elution by using the mobile phase of methanol-water(0.1%formic acid). The flow rate was 0.3 mL·min-1. Triple quadrupole mass spectrometry, electrospray ionization source (ESI),DMRM mode, and positive and negative ions alternate mode were adopted. Result: The 12 reference substances had a good specificity. Wogonoside,baicalin,wogonin,chrysin,uteolin,caffeic acid,acetylcorynoline,corynoline,protopine,salicylic acid,uracil and adenosine showed good linear relationships within the range of 0.062 24-16.24,33.95-530.4,0.013 64-3.558,0.001 157-0.302 4,0.001 199-0.313 0,0.014 64-3.821,0.000 739 5-0.038 59,0.060 83-3.174,0.002 443-0.637 4,0.021 80-1.138,0.022 99-6.000,0.006 046-1.578 μg·L-1,with a good precision,stability and repeatability. And the average recoveries were 98.9%,100.2%,106.9%,100.8%,101.7%,99.3%,94.6%,100.0%,100.5%,103.4%,96.8%,98.1%. Conclusion: This method was simple,sensitive and reliable. It laid a foundation to promote the quality control standard of Pudilan Xiaoyan oral liquid.

Article in Chinese | WPRIM | ID: wpr-774519


UPLC-ESI-Orbitrap-MS/MS was used to analyze,identify and attribute the chemical constituents in Pudilan Antiphlogistic Oral Liquid. The analysis was performed on an Agilent Eclipse XDB-C18(4.6 mm × 150 mm,3.5 μm) with a gradient mobile phase of methanol-0.1% formic solution system at the flow rate of 0.5 m L·min-1. The sample volume was 2 μL. The column temperature was30 ℃. The high-resolution orbitrap mass spectrometry was used as detector,with electrospray ion source in both positive and negative models,and the MS scanning ranged between m/z 50 and 2 000. Based on the analysis of mass spectrometry and literature reports,79 compounds were confirmed,including 30 alkaloids,28 organic acids,18 flavonoids and 3 coumarins. Finally,39 compounds,such as rutin,esculetin,gallic acid,caffeic acid,cichoric acid,were identified from Taraxacum mongolicum; 11 compounds,such as baicalin,baicalein,apigenin,chrysin,oroxylin A,were identified from Scutellaria baicalensis; 13 compounds,such as arginine,proline,hypoxanthine,epigoitrin,indirubin,were identified from Isatis indigotica; and 18 compounds,such as dehydrocheilanthifoline,oxysanguinarine,corynoline,protopine,spallidamine,were identified from Corydalis bungeana. After the analysis of chemical model and attribution,the contents of some compounds were high in Pudilan Antiphlogistic Oral Liquid,such as baicalin,wogonoside,baicalein,wogonin,apigenin,chrysin,skullcapflavonⅡ,oroxylin A,cichoric acid,chlorogenic acid,caffeic acid,esculetin,dehydrocheilanthifoline,dihydrosanguinarine,protopine,corynoline and indirubin. The established method is simple,accurate,rapid,sensitive and reproducible,and thus suitable for the qualitative identification and quantitative determination of Pudilan Antiphlogistic Oral Liquid,which lays a foundation for the systematic quality control and the establishment of whole-course traceability system of active ingredients.

Anti-Inflammatory Agents , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Chemistry , Phytochemicals , Tandem Mass Spectrometry
Article in Chinese | WPRIM | ID: wpr-687354


To study the pharmacokinetics of active ingredients (alkaloids, iridoids and flavonoids) in Huanglian Jiedu decoction (HLJDD) in Alzheimer's disease (AD) model rats, and investigate its mechanism in treatment of AD. All of rats were divided into normal control group (=6), shame operation group (=6) and model group (=12). Rats in shame operation group received daily subcutaneous injection of D-galactose (D-gal 50 mg·kg⁻¹) for a total of 45 d to induce subacute aging model. Based on the operation of shame operation group, the rats in model group were given with an injection of Aβ₂₅₋₃₅ (4.0 g·L⁻¹)-ibotenic acid (2.0 g·L⁻¹) into the nucleus basalis magnocellularis. Then rats in model group were divided into HLJDD one day administration group (=6) and HLJDD one week group (=6). The plasma concentration of alkaloids, iridoid and flavonoids was determined by liquid chromatography tandem mass spectrometry (LC-QQQ-MS) at different time points. The levels of seven inflammatory factors (MIP-2, IL-1β, IL-2, IL-8, IL-10, IL-13, TNF-α) in cerebrospinalfluid (CSF) were measured by Bio-Plex multi-factor detection technology. Iridoids in AD model rats, with high bioavailability, were easily absorbed and eliminated. The plasma concentration of alkaloid was lower, and the AUC (area under the curve) was higher in HLJDD one week group than that in HLJDD one day group. The plasma concentration-time curves of flavonoids showed obvious bimodal phenomena. After the gastric administration of HLJDD, the inflammatory factors in CSF of AD rats demonstrated a callback trend, including IL-1β/IL-10 (<0.05) with significant difference. The pharmacokinetic behaviors of iridoids, alkaloids and flavonoids (41 compounds) in AD model rats were fundamentally elucidated, and HLJDD can improve the central inflammatory status of AD rats by regulating the levels of inflammatory factors.