RESUMO
This work describes the holistic fingerprinting method based on liquid chromatography coupled with charged aerosol detection(CAD) to profile non-saponin from water-soluble parts and determination of dencichine in Panax ginseng(PG), P. quinquefolium(PQ) and P. notoginseng(PNG). Sample extraction was carried out by water with ultra sonication for 30 min, which was eluted by Retain PEP for further analysis. The analysis was performed on a Hypercarb of porous graphitized carbon(3.0 mm×150 mm, 3 μm) column with acetonitrile and 0.1% perfluoropentanoic acid as mobile phase at a flow rate of 0.8 mL·min~(-1). Temperature of evaporator and nitrogen pressure for CAD were set at 50 ℃and 60.1 psi(1 psi≈6.895 kPa), respectively. As a result, dencichine and other polar components had a good performance on resolution and retention. The correlation coefficient(R~2) of dencichine was 0.998 2 in the concentration from 0.019 2 to 0.48 μg·mL~(-1). Limit of quantitation calculated by signal to noise of 10 was 7.4 ng·mL~(-1), and the recovery ranged from 95.52% to 102.7%. Chemical profile of the water-soluble part from PG, PQ and PNG was similar holistically, while the relative content for dencichine and other partial components varied significantly. The proposed method was used for characteristic of chemical profiling for non-saponin from water-soluble part, and determination of dencichine in PG, PQ and PNG.
Assuntos
Aerossóis , Diamino Aminoácidos , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Panax , Panax notoginseng , Raízes de Plantas , Saponinas , ÁguaRESUMO
Aryloxypropanolamine is an essential structural scaffold for a variety of β-adrenergic receptor antago-nists such as metoprolol. Molecules with such a structural motif tend to degrade into α, β-hydroxypropanolamine impurities via a radical-initiated oxidation pathway. These impurities are typically polar and nonchromophoric, and are thus often overlooked using traditional reversed phase chromatography and UV detection. In this work, stress testing of metoprolol confirmed the generation of 3-isopropylamino-1,2-propanediol as a degradation product, which is a specified impurity of metoprolol in the European Pharmacopoeia (impurity N). To ensure the safety and quality of metoprolol drug products, hydrophilic interaction chromatography (HILIC) methods using Halo Penta HILIC column (150 mm×4.6 mm, 5 μm) coupled with charged aerosol detection (CAD) were developed and optimized for the separation and quantitation of metoprolol impurity N in metoprolol drug products including metoprolol tartrate injection, metoprolol tartrate tablets, and metoprolol succinate extended-release tablets. These HILIC-CAD methods were validated per USP validation guidelines with respect to speci-ficity, linearity, accuracy, and precision, and have been successfully applied to determine impurity N in metoprolol drug products.
RESUMO
A size exclusion chromatography method ( SEC) was established for the screening of macromolecules in traditional Chinese medicine (TCM) injections. In the experiment, TCM was collected through 0. 45μm hybrid filter and separated by SEC with MAbPac SEC-1 column. Acetonitrile was added by post-column mode with a flow rate of 0. 2 mL/min to enhance the detection sensitivity, and 25 mmol/L ammonium formate was used as the mobile phase at flow rate of 0. 2 mL/min. The charged aerosol detection was carried out with Dextran and Tween as the reference standards. The molecular weight distribution of Dextran ranged from 2500 to 133800 had a good linear relationship with the retention time. No macromolecules were detected out in the selected traditional Chinese medicine injections except Kuhuang injections.
RESUMO
AIM@#Variation in structure-related components in plant products prompted the trend to establish methods, using multiple or total analog analysis, for their effective quality control. However, the general use of routine quality control is restricted by the limited availability of reference substances. Using an easily available single marker as a reference standard to determine multiple or total analogs should be a practical option.@*METHOD@#In this study, the Ultra-HPLC method was used for the baseline separation of the main components in ginseng extracts. Using a plant chemical component database, ginsenosides in ginseng extracts were identified by Ultra-HPLC-MS analysis. The charged aerosol detection (CAD) system with post-column compensation of the gradient generates a similar response for identical amounts of different analytes, and thus, the content of each ginsenoside in ginseng extracts was determined by comparing the analyte peak area with the reference standard (determination of total analogs by single marker, DTSM). The total ginsenoside content was determined by the summation of reference standard and other ginsenoside components.@*RESULTS@#The results showed that DTSM approaches were available for the determination of total ginsenosides in a high purity ginseng extract because of the removal of impurities. In contrast, DTSM approaches might be suitable for determination of multiple ginsenosides without interference from impurities in the crude ginseng extract.@*CONCLUSION@#Future practical studies similar to the present study should be conducted to verify that DTSM approaches based on CAD with post-column inverse gradient for uniform response are ideal for the quality control of plant products.