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Method for detecting buspirone and metabolites thereof through LC_MS_MS

A metabolite, buspirone technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as imperfections, achieve the effects of small sample size, short time, and improved detection efficiency

Pending Publication Date: 2021-09-03
BEIJING HARMONY HEALTH MEDICAL DIAGNOSTICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is not perfect to only monitor buspirone and / or 1-(2-pyrimidinyl)-piperazine in blood (Wu Jingyan, et al. Heilongjiang Medicine, 2004(4); Du Qing, et al. Journal of Pharmaceutical Analysis, 2003(23))

Method used

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  • Method for detecting buspirone and metabolites thereof through LC_MS_MS
  • Method for detecting buspirone and metabolites thereof through LC_MS_MS
  • Method for detecting buspirone and metabolites thereof through LC_MS_MS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Example 1 Detection of buspirone and its metabolites

[0077] 1. Preparation of standard working solution

[0078] 1. Prepare standard solutions containing buspirone, 6-hydroxybuspirone and 1-(2-pyrimidinyl)-piperazine. The concentrations of the three targets are 1ng / mL and 4ng / mL , 10ng / mL, 40ng / mL, 100ng / mL, 200ng / mL and 400ng / mL seven serial standard solutions.

[0079] 2. Prepare internal standard solution: Mixed isotope internal standard solution of buspirone-d8, 6-OH-buspirone-d8 and 1-(2-pyrimidinyl)-piperazine-d8 with a concentration of 40ng / mL standard solution.

[0080] 3. Take seven centrifuge tubes, add 10 μL of the above-mentioned seven different concentrations of standard solutions, add 10 μL of mixed isotope internal standard solution, add methanol:water (V:V)=70:30 mixed solvent 100 μL and mix well. Get seven standard working solutions with different concentrations for later use.

[0081] 2. Pretreatment of blood samples

[0082] 1. Take 2 mL of the...

Embodiment 2

[0133] Embodiment 2 Determination of limit of quantification and limit of detection

[0134] A blank serum sample containing no target substance was used to add a standard to prepare a standard containing buspirone (0.1ng / mL), 6-hydroxybuspirone (0.1ng / mL) and 1-(2-pyrimidinyl)- Piperazine (0.1ng / mL) blood samples were diluted to different degrees with blank serum samples to prepare blood samples diluted 2 times, 3 times, 4 times, and 5 times respectively, and 10 μL of mixed isotope internal standard solution was added. Subsequent processing is the same as the above blood sample pretreatment process, and the determination is carried out according to the LC_MS_MS detection conditions determined above. The limits of detection and quantitation for buspirone, 6-hydroxybuspirone, and 1-(2-pyrimidinyl)-piperazine are shown below:

[0135] Buspirone:

[0136] (1) Limit of detection (LOD): 0.02ng / mL, S / N=5.4.

[0137] (2) Limit of quantification (LOQ): 0.03ng / mL, S / N=14.6.

[0138...

Embodiment 3

[0145] Embodiment 3 The mensuration of rate of recovery and precision

[0146] The standard working solutions of buspirone, 6-hydroxybuspirone and 1-(2-pyrimidinyl)-piperazine were prepared respectively to concentrations of 0.4 ng / mL, 4.0 ng / mL, 20 ng / mL and 32 ng 4 kinds of concentrations / mL carry out sample addition recovery rate and precision experiment, measure by the LC_MS_MS method among the embodiment 1, measure 4 samples in parallel, buspirone, 6-hydroxybuspirone, 1-(2- The recovery and precision of pyrimidinyl)-piperazine are shown in Table 7.

[0147] Table 7 Buspirone, 6-hydroxybuspirone, 1-(2-pyrimidinyl)-piperazine spiked recoveries

[0148]

[0149] It can be seen from Table 7 that the precision of buspirone, 6-hydroxybuspirone and 1-(2-pyrimidinyl)-piperazine in the concentration range of 4 different levels is 0.61% ~ 2.63%, and the average recovery The rate is 99.50% ~104.75%, the precision is high, and the recovery rate of the standard addition is good, so ...

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Abstract

The invention belongs to the technical field of drug detection, and particularly discloses a method for detecting buspirone and metabolites thereof through LC_MS_MS. The method comprises the following steps: determining LC conditions, determining MS conditions, and detecting a sample to be detected according to the determined LC conditions and MS conditions. The method provided by the invention at least has one of the following beneficial effects: the method provided by the invention can be used for determining one, two or three of buspirone, 6-hydroxy buspirone and 1-(2-pyrimidyl)-piperazine. When buspirone, 6-hydroxy buspirone and 1-(2-pyrimidinyl)-piperazine are detected at the same time, the required sample size is small, the analysis time is shortened, the detection efficiency is improved, and large-scale detection is facilitated.

Description

technical field [0001] The application belongs to the technical field of drug detection, more specifically, it relates to a method for detecting buspirone and its metabolites by LC_MS_MS. Background technique [0002] Buspirone belongs to the azaspirocyclodecanedione class of anxiolytic drugs, and exerts curative effect by reducing the effect of serotonin neurotransmitter. It has the advantages of good clinical application effect, small side effects, and no addiction. An ideal anti-anxiety drug. Buspirone is mainly metabolized in two ways in the body. One way is to generate the active metabolite 6-hydroxybuspirone through hydroxylation (Dockens RC, Salazar DE, Fulmor IE et al. Journal of Clinical Pharmacology, 2006; 46:1308), and another pathway is through oxidative dealkylation to form the active metabolite 1-(2-pyrimidinyl)-piperazine. [0003] Clinically, the dosage of buspirone is small, and its blood concentration is low due to the first-pass effect of the liver. The ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04G01N30/06G01N30/12G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/482G01N2030/484G01N30/02G01N30/06G01N30/12G01N30/04G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8679G01N2030/045G01N2030/065G01N2030/3007G01N2030/324
Inventor 贾永娟刘春冉倪君君
Owner BEIJING HARMONY HEALTH MEDICAL DIAGNOSTICS CO LTD
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