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Qualitative and Quantitative Determination of Bioactive Phytochemicals in Selected Cassia Species Using HPLC-ESI-QTOF-MS and UPLC-ESI-QqQLIT-MS/MS
Published in Brijesh Kumar, Vikas Bajpai, Vikaskumar Gond, Subhashis Pal, Naibedya Chattopadhyay, Phytochemistry of Plants of Genus Cassia, 2021
Brijesh Kumar, Vikas Bajpai, Vikaskumar Gond, Subhashis Pal, Naibedya Chattopadhyay
The system used was an Acquity ultra-performance liquid chromatography (UPLC) consisting of an autosampler and a binary pump (Waters, Milford, MA) equipped with a 10 µL loop (partial loop injection mode). The UPLC system was coupled to triple-quadrupole linear ion trap mass spectrometer (API 4000 QTRAP™ MS/MS system from AB Sciex, Concord, ON, Canada) equipped with electrospray (Turbo VTM) ion source was operated in negative ionization mode.
The Precision Medicine Approach in Oncology
Published in David E. Thurston, Ilona Pysz, Chemistry and Pharmacology of Anticancer Drugs, 2021
The analytical platforms used for measuring metabonomics are based on NMR and mass spectrometry (MS), usually combined with various forms of chromatographic separation. The evolution of these technologies has allowed metabonomics to become a useful tool in drug development. In practice, the main two techniques used are NMR and LC-MS. In particular, Ultra Performance Liquid Chromatography combined with MS (UPLC-MS) is a particularly useful methodology due to its superior resolution and speed. Although NMR and LC-MS approaches have different strengths and weaknesses, they complement each other effectively. While NMR allows the identification and quantitation of mainly small polar molecules, LC-MS has advantages for profiling larger nonpolar molecules. Also, NMR requires little sample preparation, allows rapid profiling within <5 minutes per sample and is directly quantitative. However, LC-MS is more sensitive, can cover a wider range of metabolites, and public databases are available for peak matching. There is also a technique known as “statistical heterospectroscopy” (SHY) which involves the statistical combination of data obtained from both NMR and LC-MS which allows the identification of additional relevant molecules not identified by each method separately.
Performance Testing
Published in Marc B. Brown, Adrian C. Williams, The Art and Science of Dermal Formulation Development, 2019
Marc B. Brown, Adrian C. Williams
Experimental design can be influenced by the method of detection for the permeant traversing through the membrane. Most commonly, chromatographic methods such as LC-MS/MS, HPLC, or ultra-performance liquid chromatography (UPLC) are selected for analysing the permeant in the receptor fluid, or in extracts (washings) of the membrane. Chromatographic methodologies have significant advantages over other methods of detection/analysis in that the methods are versatile and can be adapted to many or most permeants traversing the skin by appropriate selection of columns, mobile phases, and detectors. In addition, multiple components from formulations permeating through the membrane can be analysed simultaneously and the methods currently available are relatively rapid and easy to use (for example, using auto-sample injectors). Importantly, from analysis of retention times, chromatographic methods measure what species has actually come through the membrane rather than what species was placed onto the membrane; biotransformations (metabolism) can occur during permeation through viable skin. One disadvantage with chromatographic methods (especially HPLC) arises as a result of the relatively low amounts of the drug permeating across the skin which can lead to problems with accurate detection and quantification, especially when components of the skin can interfere with the analysis. Methods are available to remove such contamination from the samples, for example, using pre-columns, solid phase extraction columns, solvent precipitation, or reconstitution. However, such further sample preparation can introduce errors within the analysis.
Injection of YiQiFuMai powder protects against heart failure via inhibiting p38 and ERK1/2 MAPKs activation
Published in Pharmaceutical Biology, 2022
Yongwei Nie, Yanxin Zhang, Zhi Li, Meixu Wan, Dekun Li
The quality of YQFM was confirmed by high-performance liquid chromatography connected with a mass spectrometer (HPLC–MS) analysis. The ultra performance liquid chromatography (UPLC) analysis was carried out on Waters ACQUITYTM UPLC I-Class system (Waters, Milford, MA). The chromatographic separation was carried out on a Waters Symmetry C18 column (4.6 mm × 259 mm, 5 μm). The column temperature was set at 30 °C. The mobile phase flow rate was set at 1.0 mL/min, and the injection volume was 10 μL for each run. The mobile phase and line gradient program were handled as reported previously (Zhang et al. 2019b). The MS analysis was carried out by a Waters SYNAPT G2-SI MS system (Waters, Milford, MA). The analysis parameters were set as follows: the capillary voltage was 3.0 kV and the cone voltage was set at 40 V; the source temperature was 110 °C, and the desolvation gas temperature was 350 °C; the cone gas flow was 50 L/h, and the desolvation gas flow was 800 L/h. The MS data were acquired by Waters MassLynx V4.1 software and processed by UNIFI™ 1.8 software.
Dissolving microneedles for transdermal delivery of huperzine A for the treatment of Alzheimer's disease
Published in Drug Delivery, 2020
Qinying Yan, Weiwei Wang, Jiaqi Weng, Zhenghan Zhang, Lina Yin, Qingliang Yang, Fangyuan Guo, Xingang Wang, Fan Chen, Gensheng Yang
Prior to analysis, frozen samples were thawed at 37 °C in a water bath and vortexed briefly. For the analysis, 20 μL internal standard of Hup A methanol solution (1 μg/mL), 100 μL sodium hydroxide solution (1 mol/L), and 5 mL re-distilled dichloromethane solution were added into the samples. After centrifugation at 5500 rpm for 10 min and vortex mixing for 5 min, the organic phase was transferred to another glass tube and evaporated to dryness at 40 °C under a gentle stream of nitrogen. The residue was reconstituted in 100 μL methanol, and centrifugation at 10,000 rpm for 5 min, then the supernatant was collected and injected into the LC–MS system. The separation was performed using a Waters HSS T3 column (100 mm × 2.1 mm, 1.8 μm) in an AcquityTM ultra performance liquid chromatography (UPLC) system. Acetonitrile and water containing 0.1% of formic acid (60:40 v/v) were used as mobile phase A and mobile phase B, respectively. The flow rate was 2.0 μL/min. The temperature for the column was 30 °C. The analyte was quantified using a Waters XEVO TQ-S micro triple quadrupole mass spectrometer equipped with an electro-spray ionization (ESI) source. Multiple reactions monitoring (MRM) scan type was used in the positive scan mode to increase the specificity of the analysis.
Development of a stability-indicating UPLC method for determination of isotretinoin in bulk drug
Published in Pharmaceutical Development and Technology, 2019
Shih-Liang Hsi, Peter Surman, Raida Al-Kassas
In contrast to HPLC, ultra-performance liquid chromatography (UPLC) is functionally advanced in its rapidness, sensitivity, and resolution (Nováková et al. 2006a). It can withstand much higher back pressure with smaller packed column, lower injection volume, and shorter run time (Nováková et al. 2006a,b). UPLC Technology is able to provide numerous benefits to routine testing of commercialised drug products, with increased sample throughput and decreased solvent consumption (Stephen et al. 2006; Wu et al. 2008). This indicates that an analytical testing method using UPLC may offer significant cost effectiveness by analysing more samples per system in lesser time. The overall operating expense in both development and quality control thus can be reduced with increased productivity. All these advantages over conventional HPLC has allowed UPLC to gain its place and popularity in the industry for both routine and research purpose nowadays (Pratima and Zibran. 2013). It is thus highly desirable to develop and validate an UPLC method for isotretinoin with satisfactory resolution, sensitivity, and relatively short analysis run time in line with routine analysis for quality control purposes. To the best of our knowledge, there is no published work that involves the development of an analytical method for quantification of isotretinoin using UPLC. Therefore, the aim of the present work was to develop and validate a stability indicating method for isotretinoin using UPLC method.