Method for detecting flumequine enantiomer in human plasma

A technology of flumequine and enantiomers, which is applied in the field of rapid and efficient detection of flumequine enantiomers in human plasma, can solve the problems of high cost, long separation time, and low precision of flumequine enantiomers, and achieve environmental Friendly, linear relationship, high precision effect

Active Publication Date: 2016-10-05
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a fast, high precision, simple operation and low cost in order to solve the defects of high cost, long separation time, narrow applicability, complicated operation and low precision in the detection of flumequine enantiomers by the existing crystallization method. Lower method for detection of flumequine enantiomers in human plasma

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Embodiment 1

[0028] A method for detecting flumequine enantiomers in human plasma, comprising the following steps:

[0029] 1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%: 10% as a mobile phase to dissolve and dilute flumequine to a solution of 40 μg / mL, and obtain a flumequine solution after filtering with a microporous membrane Standby: Weigh 1mg of propranolol standard substance, use a mixture of isopropanol and n-heptane with a volume ratio of 70%:30% to make up to 100mL, obtain a propranolol solution after ultrasonication for 10min, and store it at 4°C for future use ;

[0030] 2) Take the adult plasma and place it in a centrifuge tube, add the flumequine solution prepared in step 1), the ratio of solid to liquid is 1mL: 120mL, add anhydrous copper sulfate and monoethanolamine after shaking, centrifuge at 8000rpm for 10min, and take the supernatant , the residue was dissolved with monoethanolamine and centrifuged, the supernatant was combined, 1 / 2 volume of ...

Embodiment 2

[0035] A method for detecting flumequine enantiomers in human plasma, comprising the following steps:

[0036]1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%: 10% as a mobile phase to dissolve and dilute flumequine to a solution of 45 μg / mL, and obtain a flumequine solution after filtering with a microporous membrane Standby: Weigh 1mg of propranolol standard substance, use a mixture of isopropanol and n-heptane with a volume ratio of 70%:30% to make up to 100mL, obtain a propranolol solution after ultrasonication for 10min, and store it at 4°C for future use ;

[0037] 2) Take adult plasma and place it in a centrifuge tube, add the flumequine solution prepared in step 1), the ratio of solid to liquid is 1mL: 130mL, add anhydrous copper sulfate and monoethanolamine after shaking, centrifuge at 10000rpm for 12min, and take the supernatant , the residue was dissolved with monoethanolamine and centrifuged, the supernatant was combined, 1 / 2 volume of prop...

Embodiment 3

[0042] A method for detecting flumequine enantiomers in human plasma, comprising the following steps:

[0043] 1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%: 10% as a mobile phase to dissolve and dilute flumequine to a solution of 50 μg / mL, and obtain a flumequine solution after filtering with a microporous membrane Standby: Weigh 1mg of propranolol standard substance, use a mixture of isopropanol and n-heptane with a volume ratio of 70%:30% to make up to 100mL, obtain a propranolol solution after ultrasonication for 10min, and store it at 4°C for future use ;

[0044] 2) Take adult plasma and put it in a centrifuge tube, add the flumequine solution prepared in step 1), the ratio of solid to liquid is 1mL:150mL, add anhydrous copper sulfate and monoethanolamine after shaking, centrifuge at 12000rpm for 10-15min, take the above The supernatant and the residue were dissolved with monoethanolamine and centrifuged, combined the supernatant, added 1 / 2 vo...

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Abstract

The invention relates to a method for detecting flumequine enantiomer in human plasma. The method comprises the following steps: preparing a standard flumequine solution, adding the flumequine solution into the human plasma, and then detecting by using UFLC-MS/MS. According to the method, a solid phase extraction condition is optimized, so that the solid phase extraction time is shortened, and the efficiency is higher; the precision of the UFLC-MS/MS for analyzing the concentration of the flumequine enantiomer is high, the speed is high, the operation is simple, and the cost is relatively low; the detection method is good in linear relation to a target compound, the yield is high, the relative deviation is small, and a used reagent is low in toxicity, less in use amount and environmentally friendly.

Description

technical field [0001] The invention relates to a method for rapidly and efficiently detecting flumequine enantiomers in human plasma. Background technique [0002] Flumequine (FLU) is a second-generation fluoroquinolone antibacterial drug, which is a special antibacterial drug for animals. And aquatic animal diseases have good curative effect. Its mechanism of action is mainly to inhibit the A subunit of DNA gyrase and destroy its activity. As a result, the synthesis of deoxyribonucleic acid, ribonucleic acid and protein is disturbed, so that cells can no longer divide, thus playing a bactericidal effect. Because flumequine has high safety, tolerance and unique high permeability. Studies have found that high doses of flumequine can cause abnormal development of rat embryos. Although the harm of low doses of flumequine to humans has not been reported, the potential risk of long-term intake of food with flumequine residues cannot be underestimated. [0003] Flumequine is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 杨立业胡兆红欧阳小琨王阳光金如娜刘超王南
Owner ZHEJIANG OCEAN UNIV
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