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A method for detecting the content of optical isomers of trutroban

A technology of optical isomers and trutroban, applied in measuring devices, scientific instruments, instruments, etc., can solve difficult problems, achieve low detection limit, save manpower and material resources, and improve sensitivity

Active Publication Date: 2019-08-30
大连润生康泰医学检验实验室有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for different separation objects, it is necessary to optimize and screen a large number of conditions and parameters such as sample volume, column temperature, eluent (i.e. mobile phase), flow rate, precursor ion / product ion selection, collision energy, and cone voltage. , not only to ensure the separation of optical isomers, but also to meet the detection requirements of trace or trace drugs, which is extremely difficult

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  • A method for detecting the content of optical isomers of trutroban

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The concentration detection of racemic trutroban in the plasma of embodiment 1

[0026] The method for quantitatively detecting the content of trutroban optical isomers based on chiral high-performance liquid chromatography-mass spectrometry / mass spectrometry technology, racemic trutroban as an example, but the scope of protection of the present invention is not limited to this experiment, The specific steps are as follows: 1) preparation of samples; 2) determination of chiral chromatographic separation conditions; 3) determination of mass spectrometry conditions; 4) determination of optical isomer content.

[0027] 1. Sample preparation

[0028] ①Collection of biological samples: Take 100 μL of plasma from SD rats (5 mg / kg, intragastric administration) administered with racemic trutroban (1 hour after blood collection);

[0029] ② Add 400 μL of acetonitrile to the above biological sample, spin for 30 s, centrifuge at 12500 rpm for 10 min, take the supernatant and dry ...

Embodiment 2

[0050] Concentration detection of (R)-trutroban in the urine of embodiment 2

[0051] Except following conditions, other conditions are identical with embodiment 1:

[0052] ①Collection of biological samples: take 100 μL of urine (24h total urine) from SD rats injected with (R)-Trutroban;

[0053] ②Column: Daicel IA chromatographic column (150mm*4.6mm*5μm);

[0054] 3. The mobile phase is a mixed solution of methanol: water=80:20 (volume ratio) (containing 0.5% acetic acid and 1mM ammonium acetate by volume fraction), and the flow rate is 1mL / min, isocratic elution;

[0055] ④ Automatic sample injection, volume 10μL;

[0056] ⑤Cone voltage is 30V;

[0057] ⑥The collision energy is 50eV;

[0058] ⑦ The dwell time is 0.16s;

[0059] ⑧ESI ion source temperature is 130℃;

[0060] ⑨N 2 (Dry gas) temperature and flow rate are 450°C and 400L / h;

[0061] ⑩The capillary voltage is 2.0KV;

[0062] In this embodiment, the retention time of (R)-trutroban and (S)-trutroban is re...

Embodiment 3

[0063] The concentration detection of (S)-trutroban in the heart of embodiment 3

[0064] Except following conditions, other conditions are identical with embodiment 1:

[0065] ①Collection of biological samples: take 0.1 g of the heart of SD rats injected with (S)-trutroban (the neck was cut off 12 hours after administration, and the heart was quickly dissected out);

[0066] Preparation of homogenate: add 0.5 mL of PBS buffer solution to the biological sample, homogenize at 4 °C, and take 100 μL of supernatant after centrifugation;

[0067] Add 400 μL of acetonitrile to the above homogenate, swirl for 30 s, centrifuge at 12,500 rpm for 5 min, take the supernatant and dry it with nitrogen at room temperature to obtain the sample to be analyzed;

[0068] ②Column: Daicel IB column (150mm*4.6mm*5μm);

[0069] ③The mobile phase is a mixture of acetonitrile:water=60:40 (volume ratio) (containing 0.5% trifluoroacetic acid and 0.1mM ammonium bicarbonate by volume fraction), and ...

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Abstract

The invention provides a method for determining the content of a Terutroban optical isomer. The method specifically comprises the following steps: (1) preparing a sample; (2) determining chiral chromatographic separation conditions; (3) determining spectrometry conditions; and (4) determining the content of the optical isomer. Based on a combined high performance liquid chromatography-mass spectrometry / mass spectrometry technique, the method has the characteristic of simplicity in operation, accuracy in quantification and low batch cost and is particularly suitable for requirements of clinical drug detection / monitoring, and a novel thought and method are provided for the in-vivo / vitro detection of the Terutroban optical isomer.

Description

technical field [0001] The invention relates to a method for detecting and monitoring the content of (R)-trutroban and (S)-trutroban optical isomers in biological samples based on chiral high performance liquid chromatography-mass spectrometry / mass spectrometry, It belongs to the field of drug analysis. Background technique [0002] As early as the early 20th century, it was discovered that different chiral drug enantiomers have different properties. Through in-depth research on chiral drugs, its research methods and technologies have been developed rapidly, people have a deeper understanding of the pharmacological activities of chiral drugs, and in just a few decades, more new hand drugs have been introduced Drugs are used clinically. At present, most of the commonly used drugs are chiral molecules, especially more than 99% of the chiral drugs in natural and semi-synthetic drugs, and most of them exist in the form of a single enantiomer. However, chiral drugs account for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陈福欣严贝贝刘静加晓丹陈苏英龚频
Owner 大连润生康泰医学检验实验室有限公司