scholarly journals Ultrahigh Performance Liquid Chromatography–Electrospray Ionization Tandem Mass Spectrometry Method for Qualitative and Quantitative Analyses of Constituents of Corydalis bungeana Turcz Extract

Molecules ◽  
2019 ◽  
Vol 24 (19) ◽  
pp. 3463
Author(s):  
Miao Tian ◽  
Chunjuan Yang ◽  
Jing Yang ◽  
Hongrui Dong ◽  
Lu Liu ◽  
...  

In this study, the constituents of a Corydalis bungeana Turcz extract were qualitatively analyzed using gradient elution with a mobile phase of 0.2% acetic acid and acetonitrile. We obtained comprehensive insight into the constituents of C. bungeana Turcz extracts through the quantitative analysis of 14 compounds by comparison with authentic reference standards, and tentatively identified an additional 44 compounds through electrospray ionization mass spectrometry (ESI–MS) and tandem MS detection. The separation was successfully achieved using an Agilent SB-C18 column (1.8 µm, 150 × 2.1 mm; Agilent, Santa, CA, USA). A tandem quadrupole spectrometer was operated in either full-scan mode or multiple reaction monitoring (MRM) for the qualitative and quantitative analyses of the constituents, respectively. Validation data (inter-day and intra-day combined) for accuracy and precision ranged from −4.80% to 4.73%, and 0.30% to 4.97%, respectively. An ultrahigh performance liquid chromatographic–ESI–tandem MS (UHPLC–ESI–MS/MS) method for qualitative of C. bungeana Turcz (C. bungeana) extract and the quantification of 14 alkaloids, namely, A–N, was developed and validated. Quantitative analysis involved gradient elution with a mobile phase of 0.1% acetic acid and methanol for 45 min. The separation was successfully achieved using a Waters SB-C18 column (1.8 µm, 100 mm × 2.1 mm, Waters, Milford, Massachusetts, USA). The repeatability and stability of the method also met USFDA criteria with CV values lower than 5%. The limit of detection of the 14 alkaloids ranged from 9.74 to 13.00 ng/mL, whereas the linearities of the standard curves were between 0.9991 and 0.9995. In total, 15 commercial samples from 11 different sources were analyzed.

2015 ◽  
Vol 730 ◽  
pp. 254-259 ◽  
Author(s):  
Yan Li Cong ◽  
Shen Li ◽  
Bo Chen ◽  
Hai Yan Sun ◽  
Dong Liu ◽  
...  

The focus of the study was to establish an UPLC-ESI-MS/MS method for the qualitative and quantitative determination of VLPVPR in rat plasma. The method was as follows: Protein impurities in the rat plasma samples were precipitated with methanol; A Waters Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) was adopted; the column temperature was 25°C; the mobile phase consisted of methanol-water with gradient elution at the steady flow rate of 0.3 mL·min-1; the detection wavelength was 202 nm. Mass spectrometry applied selected ion monitoring mode with m/z 255 (quantitative ion) and m/z 169 (qualitative ion). It was found that excellent linear relationship was obtained from the range of 10~200 ng·mL-1 (r=0.9991), the limit determination (LOD) of VLPVPR was 1.8 ng·mL-1, the recovery rate was 96.33%~100.76%, The inter and intre-day RSD were less than 7%. We thus conclude that a rapid and sensitive UPLC-ESI-MS/MS method was developed and validated for the determination of recombinant antihypertensive peptide VLPVPR in rat plasma. It can be applied to evaluate the pharmacokinetics of VLPVPR.


Author(s):  
N. A. Al-Abkal ◽  
E. Kh. Metwally ◽  
S. R. Alezzbawy ◽  
Kh. Y. Orabi ◽  
Sh. H. Alshammari

Aim: To compare the main and additive components of heroin trafficked in the Stateof Kuwait during 2012 with those components of heroin traded recently in the country during 2016 and 2017, and to provide a satisfactory explanation for the increase in deaths among heroin addicts during the period2011 -2018. Study Design: Selected samples of non-pure powder heroin seized in Kuwait during 2016 and 2017, with pure heroin and a set of10 pure different heroin component standards, all have been quantitatively analyzed in the Forensic Laboratories. Place and Duration of Study: All qualitative and quantitative analyses for 2016 and 2017 samples were conducted in the Forensic Laboratories of the General Department of Criminal Evidences – Ministry of Interior – State of Kuwait. Methodology: By using Gas Chromatography/Mass Spectrometry (GC/MS) to qualitative and quantitative analysis have been made on a total of hundred samples of non-pure powder heroin seized in Kuwait during the years 2016 and 2017, in addition to ten pure standards. Results: The concentration of the diacetylmorphine (active substance of heroin) in Kuwait during the year 2017 are much higher than the concentration during the year 2016. The additive substances (adulterants) for the years 2016 and 2017, are shared with the year 2012 by the component's paracetamol, caffeine and diazepam with different concentrations. But new adulterants in recent years are recorded in samples 2016 and 2017, including methamphetamine, dextromethorphan, and methylphenidate which is absent in 2016 samples. Conclusion: The concentration % of illicit heroin traded in Kuwait as diacetylmorphine has increase from 10% to 50% for year 2016, and further from 30% - 70% for year 2017, which marks identified a substantial rising in the purity of heroin. In addition, additive substances in the two years include paracetamol (acetaminophen), caffeine and diazepam, previously recorded in 2012. However, totally different new adulterates are recorded in 2016 and 2017 samples, including methamphetamine, dextromethorphan, and methylphenidate. All new three adulterates are detected in quite a few numbers of samples with methylphenidate recorded in a very low concentration of 0. 01 mg. Both new adulterates and higher purity of heroin constitute the main reasons for rising the rate of deaths between heroin addicts in recent years. Also, recent UN reports (12,18) provide evidence that the GC countries Afghanistan, Iran and Pakistan are still manufacturing and trading the above mentioned new adulterates.


The Analyst ◽  
2020 ◽  
Vol 145 (20) ◽  
pp. 6625-6631
Author(s):  
Rongkun Lin ◽  
Qiao Lu ◽  
Zheng Lin ◽  
Wei Hang ◽  
Benli Huang

We present a strategy for the coupling of laser-induced acoustic desorption (LIAD) with electrospray ionization (ESI) mass spectrometry.


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