Method for detecting imidafenacin in human plasma through HPLC-MS/MS combination

A midanacin and human detection technology, applied in the field of biological analysis, can solve the problems of unsuitable biological sample detection, unreachable blood concentration of midanacin, long analysis time, etc., and achieves low quantitative lower limit and accuracy. good, selective effect

Active Publication Date: 2019-12-10
NANJING HEALTHNICE MEDICAL TECH +1
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Problems solved by technology

[0003] At present, domestic literature only reports the technology of determining the content of midanacin by liquid chromatography. The mobile phase used is a non-volatile salt and cannot be used for mass spectrometry analysis. The limit of quantification cannot reach the plasma concentration of midanacin in the body. It takes a long time and is not suitable for the detection of large batc...

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  • Method for detecting imidafenacin in human plasma through HPLC-MS/MS combination
  • Method for detecting imidafenacin in human plasma through HPLC-MS/MS combination
  • Method for detecting imidafenacin in human plasma through HPLC-MS/MS combination

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Embodiment Construction

[0044] The detection method of the present invention is further illustrated by the following examples, but these examples do not constitute any limitation to the present invention.

[0045] Materials and Methods

[0046] 1. Instruments and reagents

[0047] High-phase liquid chromatography (Shimadzu LC-30AD series); mass spectrometry (API 5500, Applied Biosystems / Sciex); pure water meter (MilliDirectQ, Millipore); microbalance (XP6, METTLER TOLEDO); centrifuge (HeraeusMuitifuge X1R, ThermoFisher) ; Oscillator (LPD2500, LE PARD); Nitrogen blowing instrument (Organomation Microvap 11803; NG150-1A, Lept Scientific Instrument Co., Ltd.).

[0048] Acetonitrile (Merck, HPLC grade), water (ultrapure water, laboratory-made), acetic acid (Aladdin, HPLC grade), ammonium acetate (Aladdin, HPLC grade), isopropanol (Anhui Shilian Special Solvent Co., Ltd., HPLC grade), methanol (Merck, HPLC grade). Blank plasma was obtained from healthy subjects. Midanacin (TLC, Lot No.: 1418-068A1), M...

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Abstract

The invention relates to a method for detecting imidafenacin in human plasma through HPLC-MS/MS combination, and belongs to the field of biological analysis. The detection method comprises the following steps: (1) pretreatment of a human plasma sample; (2) liquid chromatography-mass spectrometry combined detection: a mobile phase A and a mobile phase B are adopted as a mixed mobile phase for gradient elution, the mobile phase A is acetonitrile, and the mobile phase B is an ammonium acetate aqueous solution; and (3) measurement of the concentration of imidafenacin in human plasma. According tothe method, with imidafenacin-d10 as an internal standard, gradient elution is carried out by adopting Waters, ACQUITY UPLC BEH C8 chromatographic columns, the deuterated internal standard and a to-be-detected object have the same retention time, chemical property and matrix effect, and the reproducibility and accuracy for detecting the concentration of imidafenacin in blood plasma are relativelygood. The method provided by the invention can be used for evaluating the bioequivalence of each dosage form of imidafenacin.

Description

technical field [0001] The invention belongs to the field of biological analysis, in particular to a method for detecting the concentration of midanacin in blood plasma by liquid mass spectrometry. Background technique [0002] Midanacin is a new type of diphenylbutyramide muscarinic M1 / M3 receptor blocker with high bladder selectivity, used for the treatment of overactive bladder (Overactive Active Bladder,OAB). It selectively acts on the muscarinic M1 and M3 receptors of the bladder, blocks the contraction of acetylcholine on the detrusor muscle, relaxes the detrusor muscle, and can significantly improve urgency, frequency, and incontinence caused by overactive bladder symptom. Overactive bladder syndrome (overactive bladder syndrome, OAB) is a common urological disease, and with voiding disorder as the clinical characteristics, mainly clinical syndromes such as frequent urination, urgency, and urge urinary incontinence. The incidence of OAB increases with age, so it has...

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/36G01N30/86
CPCG01N30/02G01N30/06G01N30/36G01N30/8679G01N2030/062G01N2030/027
Inventor 高倩倩唐胜辉王华娟
Owner NANJING HEALTHNICE MEDICAL TECH
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