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Liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine

A technology of triptolide ketone and triptolide A, which is applied in the field of biological sample inspection, can solve the problem of high weight content, and achieve the effects of high quantitative accuracy, high sensitivity and simple operation

Active Publication Date: 2015-10-21
INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Tripterygium wilfordii is a triterpenoid component of Tripterygium wilfordii, the first monomer isolated from Tripterygium wilfordii. Although it has a variety of pharmacological activities, it is the main toxic component. Stem bark content is high

Method used

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  • Liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine
  • Liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine
  • Liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 qualitative analysis

[0027] 1. Reagents

[0028] The test water of the present invention is first-class water (see GB / T 6682-2008 regulations):

[0029] a) Sodium dihydrogen phosphate, disodium hydrogen phosphate, and sodium hydroxide are analytically pure;

[0030] b) Methanol, acetonitrile, diethylamine, isopropanol, ammonium acetate, formic acid, ethyl acetate, and cyclohexane are all chromatographically pure;

[0031] c) Phosphate buffer solution (pH 5.8): Take 8.34 g of potassium dihydrogen phosphate and 0.87 g of dipotassium hydrogen phosphate, put them in a 1000 mL volumetric flask respectively, add grade 1 water to dissolve and dilute to the mark;

[0032] d) 10mM ammonium acetate containing 0.1% formic acid: weigh 0.384g of ammonium acetate, add a certain amount of first-grade water to dissolve, add 0.5mL formic acid and mix well, and dilute the mixture to 500mL with first-grade water;

[0033] e) Standard solution:

[0034] 1) Triptolide A, ...

Embodiment 2

[0094] Embodiment 2 quantitative analysis

[0095] 1, reagent is the same as embodiment 1

[0096] 2, instrument and material are the same as embodiment 1

[0097] 3. Sample extraction

[0098] Accurately measure 1.0mL-2.0mL or 1.0g-2.0g of the case sample in parallel; take two blank samples of the same matrix, and add the corresponding target standard (the amount added should be similar to the rough measurement of the case sample) to prepare Add sample, mix well. Others are the same as embodiment 1.

[0099] 4. Instrument detection is the same as in Example 1

[0100] 5. Record and calculate

[0101] 5.1. Calculate drug content

[0102] Record the peak area value of the target substance in 2 to 3 parallel injections of each sample, and calculate the content according to the formula (2):

[0103]

[0104] In the formula:

[0105] W - the content of the target substance in the sample per unit mass, in micrograms per gram (μg / g) or micrograms per milliliter (μg / mL); ...

Embodiment 3

[0121] Embodiment 3 utilizes non-fresh blood to evaluate the method of the present invention

[0122] 1, reagent, with embodiment 1.

[0123] 2, apparatus and material, with embodiment 1.

[0124] 3. Sample extraction

[0125] Take 2.0 mL of blank non-fresh blood in a stoppered test tube, add triptolide A, triptolide ketone, triptolide and triptolide standard products respectively to prepare added samples, and mix well.

[0126] A certain amount of sodium hydroxide solution was added to the above samples to adjust the pH to 9, 10.0 mL of ethyl acetate was added, shaken for 10 min, and centrifuged at high speed for 10 min. After separating the organic phase, add an organic solvent to carry out the second extraction, combine two organic phases (the inorganic phase after the second extraction is carried out to high-performance liquid chromatography analysis, the extraction rate of the sample is 99.9%), and place it in a 50°C concentrator Wipe dry. The residue was fixed to vol...

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Abstract

The invention relates to a liquid chromatography-tandem mass spectrometry test method of wilforlide, triptonide, triptolide and tripterine. The test method includes the following steps: taking liquid samples or tissue samples, cutting into pieces and placing into a tube with a stopper; adding a certain amount of a sodium hydroxide solution into the samples to adjust the pH to be 9-10, adding ethyl acetate, oscillating for 10 minutes, and performing high speed centrifugation for 10 minutes; after separation of an organic phase, adding an organic solvent for secondary extraction, mixing the two obtained organic phases, and placing on a concentrator with the temperature of 50 DEG C for evaporation until the organic phases are dried; using an initial mobile phase to dilute the residue, enabling the obtained solution to pass through a 0.22-[um]m microporous organic membrane, and taking the filtrate for analysis by a liquid chromatography-tandem mass spectrometer. The test method provided by the invention is simple, efficient, quick, sensitive, high in accuracy and extensive in practicability, can be applied to qualitative and quantitative testing for wilforlide, triptonide, triptolide and tripterine in biological samples, and is suitable for tests on in-vitro samples and suspicious physical evidences.

Description

technical field [0001] The invention belongs to the field of biological sample inspection, and in particular relates to a liquid chromatography-tandem mass spectrometry inspection method for triptolide A, triptolide ketone, triptolide and triptolide. Background technique [0002] Triptergium wilfordii Hook.f is an annual vine of the Euonymus family, and is a commonly used Chinese herbal medicine in traditional Chinese medicine. Tripterygium wilfordii is the root of the Euonymus plant Tripterygium wilfordii. Distributed in the south and southwest of the Yangtze River Basin, mainly in the middle and lower reaches of the Yangtze River. It has been reported that more than 100 components have been isolated from Tripterygium genus at present, mainly diterpenes, triterpenes, sesquiterpenes and alkaloids. Studies have shown that many components such as alkaloids and diterpenes Both active ingredients and toxic ingredients, diterpenoids are the most toxic, mainly causing severe dam...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王芳琳栾玉静应剑波姚伊人刘耀
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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