Development and Validation of Liquid Chromatography-Tandem Mass Spectrometry Method for Simple Analysis of Sumatriptan and its Application in Bioequivalence Study

Abstract

This work demonstrated a sensitive, selective, and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantitation of sumatriptan in human plasma samples. Terazosin was used as an internal standard to minimize the variability during sample processing and detection. Sample cleanup prior to chromatographic analysis was accomplished by liquid-liquid extraction (LLE) with tert-butyl methyl ether (t-BME). The separation was performed on a reversed-phase Symmetry® C18 column (150 × 4.6 mm i.d., 5 µm) under a gradient mode, using a 0.2% formic acid aqueous solution and acetonitrile at a flow rate of 0.5 mL/min. Sumatriptan (m/z 296.26→251.05) and terazosin (m/z 388.10→290.25) were quantified using a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) under the positive ion mode. The method was fully validated following US-FDA and EMA guidelines. The LC-MS/MS assay had a calibration range of 0.5–50.0 ng/mL. The assay was precise and accurate with a between-run precision of <9.51%, and between-run accuracy between −7.27 to 8.30%. The developed method was subsequently applied in the determination of plasma concentration-time profile of a sumatriptan 50-mg tablet following oral administration in healthy volunteers.

What is the role of current mass spectrometry in pharmaceutical analysis?

“…The highly sensitive detection has been recently demonstrated by UHPLC/HPLC‐QqQ methods used for the bioequivalence study of dabigatran, which is the active metabolite of the prodrug dabigatran etexilate mesylate (Abd Allah et al, 2022), triamterene and hydrochlorothiazide (Margaryan et al, 2019), sumatriptan (Wichitnithad et al, 2020), and beraprost sodium (Prasaja et al, 2019). MS is also needed when the API does not contain chromophores for UV‐VIS detection, for example, bioequivalence study of isosorbide‐5‐mononitrate (Zhou et al, 2020) or the total amount of the drug in plasma and the unbound fractions are required, for example, bioequivalence study of paclitaxel protein‐bound particles for injectable suspension (Li et al, 2019).…”

Electrochemical Sensor Based on Ni-Co Layered Double Hydroxide Hollow Nanostructures for Ultrasensitive Detection of Sumatriptan and Naproxen

“…Sumatripta (1-[3-(2-dimethylaminoethyl)-1H-indol-5-yl]-N-methylmethanesulfonamide) is one of the triptan drugs medically administrated to manage cluster headache and migraine [ 1 , 2 ]. Sumatriptan is a selective 5-hydroxytryptamine (5-HT 1B/1D ) receptor agonist [ 3 ]. Its binding with serotonin type-1D receptors leads to extensively dilated cranial vessel vasoconstriction, thus reducing migraine pain [ 4 ].…”

Two spectroscopic methods for estimation of anti‐migraine medications: Sumatriptan and Zolmitriptan based on nucleophilic substitution reaction

“…[4] Many analytical techniques have been reported for estimation of sumatriptan succinate either as a pure raw material or in pharmaceutical dosage forms including: spectrophotometry, [5][6][7][8] spectrofluorimetry, [9,10] and high-performance liquid chromatography (HPLC). [11][12][13][14][15][16][17][18] Zolmitriptan (ZOL), chemically known as (S)-4-{3-[2-(dimethylamino)ethyl]indol-5-ylmethyl}-1,3-oxazolidin-2-one (Figure 1) is an (5-HT1) agonist with similar actions and uses as SUM. The reported methods for its estimation include spectrophotometry, [8,[19][20][21] HPLC, [15,[22][23][24] liquid chromatographymass spectrometry (LC-MS) [25] and spectrofluorimetric methods.…”