Background:
Fenugreek seeds are employed in many traditional systems as an antibacterial,
antidiabetic agent, gastric stimulant, and also for anti-invasive activity. Therefore, it is a suitable bioactive
marker to establish the quality of crude drug and its formulations.
Methods:
A rapid, simple and sensitive LC-MS/MS analytical method was developed and validated for
the determination of trigonelline extracted from Trigonella foenum-graecum (L.) (Fenugreek) and marketed
dietary supplements using Etofylline as an internal standard. The objective of the present study is
to quantify Trigonelline extracted from Trigonella foenum graecum L. (fenugreek) and marketed dietary
supplements. Chromatographic separation was achieved on a Zorbax C18 column (50mm x 4.6mm i.d,
5μ particle size). The samples were eluted using 0.1% Formic acid in water: Methanol (20:80%v/v) at a
flow rate of 0.5ml/min with a runtime of 5 min. The eluents were monitored using a tandem mass spectrometer
equipped with an electro spray ionization source in positive mode.
Results:
The analysis was performed in multiple reaction monitoring (MRM) mode by quantifying the
ion transitions from m/z 138.0→92.5 (Trigonelline) and m/z 225.0→180.90 (IS). The developed method
was linear over the concentration range 5-50 ng/mL. The LOD and LOQ were found to be 1.0 ng/mL
and 10.0 ng/mL, respectively. The correlation coefficient (r2) was found to be ≥0.998 for Trigonelline.
Conclusion:
The proposed validated LC-MS/MS method offers a sensitive quantification of trigonelline in
Trigonella foenum graecum L. (fenugreek) and marketed dietary supplements containing fenugreek seeds.
Background:
Extensive therapeutic drug monitoring needs an analytical method for efficient and sensitive quantification of analytes of interest in clinical pharmacology.
Objective:
A rapid, robust, sensitive and simple UPLC-MS/MS method to quantify Methsuximide (Ms) and N-desmethyl methsuximide/Normesuximide (MsMET) in human plasma was optimized, developed, and validated for application in a pharmacokinetic study.
Method:
Reverse phased chromatography was performed using Zorbax SB-C18, 4.6 x 75 mm., 3.5 µm as stationary phase, methanol and 0.1% formic acid (60:40 v/v) as mobile phase which was delivered isocratically at a flow rate of 0.9 mL/min. The sample injection volume was 5 µL. Mass spectrometric quantification of the analytes was performed using positive electrospray ionization as mass interface along with multiple reaction monitoring (MRM) as acquisition mode.
Results:
The selected mass transition ions for analyte, metabolite and its respective internal standards are as follows, precursor ion (m/z) and product ion (m/z): Ms (204.06 and 119.02), MsMET (190.05 and 119.82), Ms internal standard (MsIS) (209.17 and 124.02), and MsMET internal standard (MsMETIS) (195.09 and 124.16), respectively. The current method was found to be linear for Ms (60.72-5920 ng/mL) and MsMET (60.38-6010 ng/mL) with r2 values not less than 0.999. The mean recoveries of all analytes ranged between 71.37 and 86.38 percentage.
Conclusion:
This method was validated in accordance with USFDA’s bioanalytical guidelines. This method could be applied for a routine analysis of Ms and MsMET in clinical pharmacological practice.
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