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.
Objectives: The aim of this present study is to develop an accurate, precise and linear Reverse-phase High-performance Liquid Chromatographic (RP-HPLC) method for the estimation of raltegravir potassium in the bulk and pharmaceutical dosage form. Methods: The chromatographic system employs a reverse phase shim-pack C 18 column, (150 x 4.6 mm; 5 μ) using the mobile phase acetonitrile: (0.05 M) ammonium acetate buffer, (pH-4 adjusted with glacial acetic acid) in the proportion of 50:50 v/v, delivered at a flow rate of 0.8 ml/min with the detection wavelength of 271 nm. Results: The developed method resulted in the retention of raltegravir at 4.31 min. Raltegravir potassium exhibited linear relationship (r 2 > 0.9999) over the analytical range 10-50 μg/ml. The precision was exemplified by a relative standard deviation of 1.60 %. The percentage recovery was found to be in the range of 100-102 %, during accuracy studies. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) was found to be 0.104 µg/ml and 0.315 µg/ml, respectively. Conclusion: An accurate, precise and linear RP-HPLC method was developed and validated for the quantitative estimation of raltegravir potassium in (20 mg, 50 mg) tablet as per ICH guidelines and hence it can be used for the routine analysis in various pharmaceutical industries.
Flibanserin, a multifunctional serotonin agonist and antagonist (MSAA), which may treat hypoactive sexual desire disorder (HSDD) in women. Women with HSDD have a chronic lack of interest in sex that cannot be explained by another medical condition. Feelings of distress also accompany HSDD. Mechanism of action of flibanserin is different because it works on a women’s brain. Flibanserin works on three necessary brain chemicals: dopamine, norepinephrine, and serotonin. It acts as a dual control model of sexual response. Various neurotransmitters, sex steroids, and other hormone effects on the sexual response with significant excitatory and inhibitory effects. Among neurotransmitters, dopamine and norepinephrine stimulate activity, while serotonin inhibits activity and the balance between before discussed systems are of significance for a healthy sexual response. By modulating serotonin and dopamine activity in some regions of the brain, flibanserin can enhance the equilibrium of sexual response balance between these neurotransmitter systems. The significant side effects of flibanserin are dizziness, sleepiness, nausea, feeling tired and trouble sleeping. Simultaneous consumption of alcohol and flibanserin may result in severely low blood pressure.
Objective: The present study is aimed to develop and validate an Ultra-Fast Liquid Chromatography-Diode Array Detector (UFLC-DAD) method for the quantification of vitamin K2 as Menaquinone-4 (MK-4) in rabbit plasma. Method: Standard solutions and spiked plasma samples of MK-4 and Internal Standard (IS) were prepared from primary stock solutions of 1mg/ ml concentration in ethanol each. Protein precipitation was carried out for the MK-4 and IS extraction from plasma spiked samples. Chromatographic separation was employed using Isopropyl Alcohol and Acetonitrile (50:50 v/v) as mobile phase and a C-18 column with 1ml/min flow rate and a run time of 10 mins. Detection was carried out in the range 190-600 nm with 269 nm set as a reference wavelength. Result: The retention times of MK-4 and IS were at 5.5 ± 0.5 mins and 8 ± 0.5 mins respectively. Calibration curve for MK-4 was found to be linear in the range of 0.374 to 6 µg/ ml with an R 2 value of 0.9934. The % RSD for accuracy was <15%, inter and intraday precisions were <10%. The samples were found to be stable throughout the study. Conclusion: This method can be applied to the estimation of MK-4 in rabbit plasma using UFLC-DAD.
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