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Method for detecting thalidomide in plasma by LC-MS/MS method

A technology of thalidomide and plasma, which is applied in the field of monitoring the drug concentration of the drug and detecting thalidomide in plasma, can solve the problem that the clinical efficacy of thalidomide has no obvious dose relationship, cannot fully meet the needs of clinical determination, and affects Thalidomide precision drug use and other issues, to achieve the effect of short analysis time, short processing time, and easy operation

Inactive Publication Date: 2017-04-26
GUANGZHOU ZHONGDA NANSHA TECH INNOVATION IND PARK +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] And thalidomide may cause adverse reactions such as peripheral neuritis, dizziness, headache and constipation in clinical use.
The relationship between its clinical curative effect, adverse reactions and the dose of thalidomide is not obvious, which significantly affects the precise drug use of thalidomide. Therefore, it is necessary to detect the blood concentration of the drug to provide a key basis for the clinical rational use of thalidomide
[0004] At present, the detection methods of thalidomide mainly include high-performance liquid chromatography and reversed-phase high-performance liquid chromatography. The former has low sensitivity and long detection time, while the latter detection methods reported in the literature still cannot fully meet the needs of clinical determination.

Method used

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  • Method for detecting thalidomide in plasma by LC-MS/MS method
  • Method for detecting thalidomide in plasma by LC-MS/MS method
  • Method for detecting thalidomide in plasma by LC-MS/MS method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Establishment of a standard curve for determining the concentration of thalidomide in plasma

[0047] 1. Preparation of standard working solution:

[0048](1) Accurately weigh 0.0100g of thalidomide standard substance, dissolve it with 1ml DMSO, transfer it into a 10ml volumetric flask, and dilute to the mark with DMSO, shake well to obtain a standard stock solution of 1 000 μg / ml, place in Store in refrigerator at -20°C. Then use methanol: acetonitrile: formic acid (50:49:1, v / v / v) solution gradient dilution to prepare standard working solutions with concentrations of 20, 50, 250, 1000, 2500, 5000, 10000, 20000 ng / ml, Store in refrigerator at 4°C.

[0049] (2) Accurately weigh 0.0050 g of umbelliferin standard substance, dissolve it in methanol, transfer it to a 50 ml volumetric flask, and measure it with methanol: acetonitrile: formic acid (50:49:1, v / v / v). Bring the volume up to the mark, shake well to obtain a 100 μg / ml standard stock solution, and stor...

Embodiment 2

[0064] Example 2 Detection of spiked samples

[0065] 1. Pretreatment of spiked plasma samples

[0066] (1) Venous blood was collected from healthy volunteers. The blood samples were placed in heparinized EP tubes, and the whole blood was centrifuged at 4000 rpm for 5 min to absorb the upper plasma, that is, the blank human plasma, which was divided into 100 µL and stored at -80°C.

[0067] Thalidomide was added to blank human plasma to obtain spiked plasma samples with thalidomide concentrations of 2, 5, 100, and 1600 ng / mL.

[0068] (2) Take 100 µL of the spiked plasma sample, and after processing according to the sample pretreatment in Example 1, take 80 µL of the supernatant and transfer it into the sample bottle.

[0069] 2. Detection of spiked plasma samples

[0070] 10 µL was injected for UPLC-MS / MS analysis, and the conditions were the same as in Example 1. According to the standard curve, the plasma sample concentration is calculated as 2.1±0.3, 5.2±0.5, 107.8±3.6...

Embodiment 3

[0072] Example 3 Sample detection

[0073] 1. Thalidomide concentration in patients with inflammatory bowel disease after taking different doses of thalidomide tablets for 12 hours

[0074] (1) About 2 mL of venous blood was collected from patients with inflammatory bowel disease after taking different doses of thalidomide tablets for 12 hours. Blood samples were placed in heparinized EP tubes, and the whole blood was centrifuged at 4000 rpm for 5 min to absorb the upper layer of plasma, which was divided into 100 µL and stored at -80°C until assayed.

[0075] (2) 100 µL of human plasma sample was pretreated with the sample pretreatment method described in Example 1, and 80 µL of the supernatant was taken and transferred into the sample bottle.

[0076] 2. Concentration study of plasma samples in patients with inflammatory bowel disease after taking different doses of thalidomide tablets for 12 hours

[0077] 10 µL was injected for UPLC-MS / MS analysis, the conditions were th...

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Abstract

The invention discloses a method for detecting thalidomide in plasma by an LC-MS / MS method, comprising the steps: firstly, precisely measuring blank plasma, adding a series of thalidomide standard operating fluid, adding sodium citrate buffer fluid and internal standard umbelliferone standard operating fluid, carrying out pretreatment by adopting a liquid-liquid extraction method, analyzing by the LC-MS / MS method to obtain the chromatogram of each sample, and establishing a standard curve by taking the peak area ratio of the substance to be detected to the internal standard as a horizontal ordinate and the concentration of the substance to be detected as a longitudinal coordinate; then precisely measuring plasma to be detected, adding an equal volume of sodium citrate buffer fluid, then adding the internal standard umbelliferone standard operating fluid, carrying out pretreatment by the liquid-liquid extraction method, carrying out LC-MS / MS analysis to obtain the chromatogram of each sample, and calculating the concentration of the sample plasma by using the standard curve. The method is simple and quick in operation and high in sensitivity, accuracy and precision, uses safe non-poisonous solvents, and can meet the requirements on monitoring the concentration of a thalidomide medicament in clinical application.

Description

technical field [0001] The invention belongs to the technical field of pharmacokinetic analysis. More specifically, it relates to a method for detecting thalidomide in plasma by using liquid phase mass spectrometry technology, which can be used for monitoring the drug concentration of the drug. Background technique [0002] Thalidomide (THD), whose trade name is Thalidomide, was launched by the German pharmaceutical company Granta in the 1950s and was widely used as a sedative and a drug to prevent vomiting of pregnancy. Later, it was caused by Thalidomide The newborn baby was withdrawn from the market due to congenital deformity of limbs, that is, the "reactin incident". Later, it was found that thalidomide can inhibit angiogenesis, inhibit tumor necrosis factor and immunosuppressive effects. At present, it is clinically used to treat leprosy erythema nodosum, multiple myeloma, rheumatoid arthritis, rheumatic diseases and refractory ulcerative colitis, etc. [0003] The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/8822G01N2030/062
Inventor 姜福林钟国平高翔黄民
Owner GUANGZHOU ZHONGDA NANSHA TECH INNOVATION IND PARK
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