scholarly journals Determination of Alkaloids and Flavonoids in Sophora flavescens by UHPLC-Q-TOF/MS

2021 ◽  
Vol 2021 ◽  
pp. 1-13
Author(s):  
Yaqian Dong ◽  
Guoxiang Jia ◽  
Jingwen Hu ◽  
Hui Liu ◽  
Tingting Wu ◽  
...  
Keyword(s):  
Chemical Constituents ◽  
Neutral Loss ◽  
Relevant Literature ◽  
Sophora Flavescens ◽  
Fragment Ions ◽  
Mobile Phases ◽  
Characteristic Fragment ◽  
Fragmentation Rules ◽  
Tof Ms

This study is based on UHPLC-Q-TOF/MS and fragment ions to achieve classification and identification of alkaloids and flavonoids in Sophora flavescens. By reviewing the available and relevant literature, the mass fragmentation rules of alkaloids and flavonoids were summarized. 0.1% formic acid water (A) and acetonitrile (B) were used as mobile phases. 37 chemical constituents were identified, including 13 alkaloids and 24 flavonoids. This research method offers a complete strategy based on the fragmentation information of characteristic fragment ions and neutral loss obtained by MS/MS to characterize the chemical composition of Sophora flavescens.

Determination of Tuaminoheptane in Doping Control Urine Samples

2007 ◽  
Vol 13 (3) ◽  
pp. 213-221 ◽  
Author(s):  
Mario Thevis ◽  
Gerd Sigmund ◽  
Anja Koch ◽  
Wilhelm Schänzer
Keyword(s):  
Drug Testing ◽  
Limit Of Detection ◽  
Urine Samples ◽  
Fragment Ions ◽  
Liquid Liquid Extraction ◽  
In Doping ◽  
Aldehydes And Ketones ◽  
Characteristic Fragment ◽  
World Anti Doping Agency

Since January 2007, the list of prohibited substances established by the World Anti-Doping Agency includes the sympathomimetic compound tuaminoheptane (1-methyl-hexylamine, 2-heptylamine). Primarily used as a nasal decongestant drug it has been considered relevant for sports drug testing due to its stimulating properties. A confirmatory gas chromatographic-mass spectrometric procedure was developed including liquid–liquid extraction and imine formation of tuaminoheptane employing various aldehydes and ketones such as formaldehyde, acetaldehyde, benzaldehyde and acetone. Extraction and derivatisation conditions were optimised for utmost efficiency and characteristic fragment ions obtained after electron ionisation allowed for a sensitive and selective analytical assay, which was validated with regard to recovery (50%), lower limit of detection (20 ng mL−1) as well as interday- and intraday precision (< 15%). The applicability to authentic urine samples was demonstrated using administration study specimens obtained from two male persons using Rhinofluimucil (tuaminoheptane hemisulfate) for intranasal application. The administered drug was detected up to 46h after repeated topical instillation of a total of approximately 3 mg.

scholarly journals Rapid Analysis of the Main Components of the Total Glycosides of Ranunculus japonicus by UPLC/Q-TOF-MS

2010 ◽  
Vol 5 (5) ◽  
pp. 1934578X1000500
Author(s):  
Wen Rui ◽  
Hongyuan Chen ◽  
Yuzhi Tan ◽  
Yanmei Zhong ◽  
Yifan Feng
Keyword(s):  
Relevant Literature ◽  
Ultra Performance Liquid Chromatography ◽  
Flavonoid Glycosides ◽  
Complex Samples ◽  
Flavonoid Aglycones ◽  
Flight Mass Spectrometry ◽  
Fragment Ions ◽  
Main Components ◽  
Acquity Uplc ◽  
Tof Ms

A rapid method for the analysis of the main components of the total glycosides of Ranunculus japonicus (TGOR) was developed using ultra-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS). The separation analysis was performed on a Waters Acquity UPLC system and the accurate mass of molecules and their fragment ions were determined by Q-TOF MS. Twenty compounds, including lactone glycosides, flavonoid glycosides and flavonoid aglycones, were identified and tentatively deduced on the basis of their elemental compositions, MS/MS data and relevant literature. The results demonstrated that lactone glycosides and flavonoids were the main constituents of TGOR. Furthermore, an effective and rapid pattern was established allowing for the comprehensive and systematic characterization of the complex samples.

Oxybuprocaine and five metabolites simultaneously determined in urine by gas chromatography and gas chromatography-mass spectrometry after extraction with Extrelut.

1987 ◽  
Vol 33 (5) ◽  
pp. 697-700 ◽  
Author(s):  
F Kasuya ◽  
K Igarashi ◽  
M Fukui
Keyword(s):  
Gas Chromatography ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Aminobenzoic Acid ◽  
Acid Metabolite ◽  
Fragment Ions ◽  
Characteristic Fragment ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract We describe a gas-liquid chromatographic (GC) method for determination of oxybuprocaine, and a gas chromatographic-mass spectrometric (GC-MS) method for simultaneous determination of four of its nine metabolites in urine. We used an Extrelut column to simply and rapidly extract oxybuprocaine and its metabolites from urine. For the GC-MS analyses, we monitored the characteristic fragment ions at m/z 353, 395, 369, 411, and 235 for 3-butoxy-4-aminobenzoic acid (metabolite 2, M-2), 3-butoxy-4-acetylaminobenzoic acid (M-3), 3-hydroxy-4-aminobenzoic acid (M-4), 3-hydroxy-4-acetylaminobenzoic acid (M-5), and methaqualone (internal standard), respectively. We quantified the glucuronide of M-2 after enzymic treatment. The assay's selectivity and reproducibility (within-day and between-day CVs less than 8% for all metabolites) make it applicable to determine oxybuprocaine and its metabolites in human urine. Mean 9-h urinary excretion of oxybuprocaine and its five metabolites from four healthy volunteers was 89.2% after a 100-mg oral dose.

Rapid characterization and determination of isoflavones and triterpenoid saponins in Fu-Zhu-Jiang-Tang tablets using UHPLC-Q-TOF/MS and HPLC-UV

2016 ◽  
Vol 8 (21) ◽  
pp. 4211-4219 ◽  
Author(s):  
Yi Tao ◽  
Yanhui Jiang ◽  
Weidong Li ◽  
Baochang Cai
Keyword(s):  
Type Ii Diabetes ◽  
High Performance ◽  
Chemical Constituents ◽  
High Performance Liquid Chromatograph ◽  
Liquid Chromatograph ◽  
Triterpenoid Saponins ◽  
Flight Mass Spectrometry ◽  
Rapid Characterization ◽  
Tof Ms

In this study, a rapid ultra-high performance liquid chromatograph coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) was used for qualitative analysis of chemical constituents in Fu-Zhu-Jiang-Tang tablets, a new six-herb preparation for treating type II diabetes.

scholarly journals Rapid Screening of Chemical Constituents in Rhizoma Anemarrhenae by UPLC-Q-TOF/MS Combined with Data Postprocessing Techniques

2017 ◽  
Vol 2017 ◽  
pp. 1-14 ◽  
Author(s):  
Lanlan Shan ◽  
Yuanyuan Wu ◽  
Lei Yuan ◽  
Yani Zhang ◽  
Yanyan Xu ◽  
...  
Keyword(s):  
Chemical Constituents ◽  
Neutral Loss ◽  
Rapid Screening ◽  
Steroidal Saponins ◽  
Chemical Research ◽  
Literature Reviews ◽  
Different Types ◽  
Fragmentation Patterns ◽  
Anemarrhena Asphodeloides ◽  
Tof Ms

Rhizoma Anemarrhenae, a famous traditional Chinese medicine (TCM), is the dried rhizome of Anemarrhena asphodeloides Bge. (Anemarrhena Bunge of Liliaceae). The medicine presents anti-inflammatory, antipyretic, sedative, and diuretic effects. The chemical constituents of Rhizoma Anemarrhenae are complex and diverse, mainly including steroidal saponins, flavonoids, phenylpropanoids, benzophenones, and alkaloids. In this study, UPLC-Q-TOF/MS was used in combination with data postprocessing techniques, including characteristic fragments filter and neutral loss filter, to rapidly classify and identify the five types of substances in Rhizoma Anemarrhenae. On the basis of numerous literature reviews and according to the corresponding characteristic fragments produced by different types of compounds in combination with neutral loss filtering, we summarized the fragmentation patterns of the main five types of compounds and successfully screened and identified 32 chemical constituents in Rhizoma Anemarrhenae. The components included 18 steroidal saponins, 6 flavonoids, 4 phenylpropanoids, 2 alkaloids, and 2 benzophenones. The method established in this study provided necessary data for the study on the pharmacological effects of Rhizoma Anemarrhenae and also provided the basis for the chemical analysis and quality control of TCMs to promote the development of a method for chemical research on TCMs.

Analysis of oxidized and chlorinated lipids by mass spectrometry and relevance to signalling

2011 ◽  
Vol 39 (5) ◽  
pp. 1233-1239 ◽  
Author(s):  
Corinne M. Spickett ◽  
Norsyahida Mohd Fauzi
Keyword(s):  
Structural Information ◽  
Neutral Loss ◽  
Oxidation Products ◽  
Inflammatory Conditions ◽  
Fragment Ions ◽  
Specific Analysis ◽  
Diagnostic Fragment ◽  
Specific Oxidation ◽  
Inflammatory Signalling

Oxidized and chlorinated phospholipids are generated under inflammatory conditions and are increasingly understood to play important roles in diseases involving oxidative stress. MS is a sensitive and informative technique for monitoring phospholipid oxidation that can provide structural information and simultaneously detect a wide variety of oxidation products, including chain-shortened and -chlorinated phospholipids. MSn technologies involve fragmentation of the compounds to yield diagnostic fragment ions and thus assist in identification. Advanced methods such as neutral loss and precursor ion scanning can facilitate the analysis of specific oxidation products in complex biological samples. This is essential for determining the contributions of different phospholipid oxidation products in disease. While many pro-inflammatory signalling effects of oxPLs (oxidized phospholipids) have been reported, it has more recently become clear that they can also have anti-inflammatory effects in conditions such as infection and endotoxaemia. In contrast with free radical-generated oxPLs, the signalling effects of chlorinated lipids are much less well understood, but they appear to demonstrate mainly pro-inflammatory effects. Specific analysis of oxidized and chlorinated lipids and the determination of their molecular effects are crucial to understanding their role in disease pathology.

scholarly journals Rapid Identification of the Chemical Components of Ilex rotunda Thunb Using UPLC-Q-TOF-MS/MS

2021 ◽  
Vol 2021 ◽  
pp. 1-16
Author(s):  
Xinxin Chen ◽  
Junmao Li ◽  
Renyikun Yuan ◽  
Youqiong Zhuo ◽  
Yangling Chen ◽  
...  
Keyword(s):  
Chemical Constituents ◽  
Neutral Loss ◽  
Sample Pretreatment ◽  
Practical Method ◽  
Chemical Components ◽  
Flavonoid Glycosides ◽  
Active Components ◽  
Triterpenoid Saponins ◽  
Ilex Rotunda ◽  
Tof Ms

Ilicis Rotundae Cortex (IRC) consists of the bark of Ilex rotunda Thunb, and its chemical constituents mainly include flavonoid glycosides, phenols, and triterpenoid saponins. In this study, a preliminary analysis was performed to identify and obtain the chemical components from IRC to better control the quality of the medicinal materials and provide a chemical basis for the study of the efficacy of the active components. Simple and efficient sample pretreatment and ultrasonic-assisted extraction methods were used to analyze the mass spectrum fragments and fracture modes in the anion mode by UPLC-Q-TOF-MS/MS. Using a two-step strategy, the neutral loss, diagnostic ions, and characteristic fragments were studied to screen diverse skeletons and substitutions, and the possible compounds were identified by comparison with databases. The representative compounds were compared with the standard, and the mass spectrogram was found to match perfectly. Thus, our findings reveal that this method is feasible and reliable and can be used to analyze the chemical components of IRC. We identified 105 compounds, including 22 triterpenoid saponins, 15 chlorogenic acids, 33 phenylpropanoids and phenylpropanosides, 3 iridoids, 1 flavonoid, 10 lignans, 12 glycosides, and 9 other compounds. This method lays the foundation for further elucidating the pharmacodynamics of IRC and provides a practical method for the identification of IRC.

Sem and X-Ray Analysis of Renal and Biliary Calculi

1976 ◽  
Vol 34 ◽  
pp. 306-307
Author(s):  
R. J. Narconis ◽  
G. L. Johnson
Keyword(s):  
Chemical Constituents ◽  
Natural State ◽  
X Ray Diffraction ◽  
Chemical Methods ◽  
X Ray ◽  
Additional Dimension ◽  
Biliary Calculi ◽  
Calculus Formation ◽  
Scanning Electron

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.

HPLC-TOF/MS in identification of chemical constituents of Fuzhengpingxiao Capsule

2013 ◽  
Vol 32 (7) ◽  
pp. 770-779
Author(s):  
Liang ZHAO ◽  
Wen-jun TIAN ◽  
Lei LU ◽  
Hai ZHANG ◽  
Xin-xia WANG ◽  
...  
Keyword(s):  
Chemical Constituents ◽  
Tof Ms
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