NDLI: Rapid and Sensitive LC−MS–MS Method for the Determination of Sarpogrelate in Human Plasma

Content Provider	Springer Nature Link
Author	Patankar, Siddheshwar Pudage, Ashutosh Joshi, Santosh S. Vaidya, Vikas V. Gomes, el A.
Copyright Year	2009
Abstract	A rapid and sensitive liquid chromatographic–tandem mass spectrometric method has been developed and validated for the estimation of sarpogrelate in human plasma. Sarpogrelate was extracted from human plasma by solid-phase extraction. Temocapril was used as the internal standard. Heated electron spray ionization mass spectrometry was performed on a TSQ Quantum Ultra MS system. The LC column was a Hypurity C18 and the mobile phase was 2 mM ammonium formate (pH 3.00 ± 0.05):acetonitrile (30:70 v/v). A flow rate of 0.250 mL min−1 was used. The quantitative analyses were carried out in the positive ion and full scan mode over the mass range m/z 60–500. The capillary, vaporiser temperatures were 325 and 200 °C respectively. The sheath gas pressure, spray voltage, collision energy and tube lense were 40, 3,500 V, 19 V, 198 V, respectively, and the mass spectra of the drugs were recorded by total ion monitoring. Retention times and characteristic mass fragments were recorded and the chosen diagnostic mass fragments were monitored in the mass chromatography mode. Signal intensities of each of the mass fragments: m/z 477 [M + H]+ for temocapril, m/z 430 [M + H]+ for sarpogrelate, were used for quantification. The calibration curves (the ratio between the peak areas as signal intensities of the drug analyzed and that of the internal standard (temocapril: m/z 477 [M + H]+) vs. the concentration of drug) exhibited linearity over the concentration range 5.00–2,500.00 ng mL−1 human plasma. The recovery and the accuracy were calculated by comparing the peak areas as the signal intensities of each mass fragment for the drug in spiked samples after solid-phase extraction from human plasma to the peak area as the signal intensity of the mass fragment of internal standard sample. The method involves a rapid solid phase extraction from plasma, simple isocratic chromatography conditions and mass spectrometric detection that enables detection up to picogram levels with a total run time of 3.0 min only. The method was validated over the range of 5.0–2,500.0 ng mL−1. The absolute recoveries for sarpogrelate (93.72%) and IS (91.42%) achieved from spiked plasma samples were consistent and reproducible.
Starting Page	671
Ending Page	676
Page Count	6
File Format	PDF
ISSN	00095893
Journal	Chromatographia
Volume Number	69
Issue Number	7-8
e-ISSN	16121112
Language	English
Publisher	Vieweg Verlag
Publisher Date	2009-03-07
Publisher Place	Wiesbaden
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Column liquid chromatography Tandem mass spectrometry Selective reaction monitoring Sarpogrelate and temocapril Measurement Science, Instrumentation Plant Sciences Biochemistry Pharmacy Organic Chemistry Analytical Chemistry
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Analytical Chemistry Biochemistry Clinical Biochemistry

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