Method for detecting sparfloxacin enantiomer in aquatic product

A technology for aquatic products and enantiomers, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of high cost of sparfloxacin enantiomers, long separation time, complicated operation, etc., and achieve the optimization of solid-phase extraction conditions. , good linear relationship, simple operation effect

Inactive Publication Date: 2016-10-26
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a rapid, high-precision, simple-to-op

Method used

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  • Method for detecting sparfloxacin enantiomer in aquatic product

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Embodiment 1

[0026] A method for detecting sparfloxacin enantiomers in aquatic products, comprising the following steps:

[0027] 1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%:10% as the mobile phase to dissolve and dilute sparfloxacin to a solution of 50 μg / mL, and filter with a microporous membrane;

[0028] 2) Put the homogenized aquatic product into a centrifuge tube, add the sparfloxacin solution prepared in step 1), the ratio of solid to liquid is 1g:150mL, add anhydrous copper sulfate and monoethanolamine after shaking, and centrifuge at 12000rpm for 15min , take the supernatant, the residue is dissolved with monoethanolamine and centrifuged, and the supernatant is combined for subsequent use; the addition of anhydrous copper sulfate is 3 times the quality of the aquatic product, and the addition of monoethanolamine is 1g of aquatic product and 20mL;

[0029] 3) Add n-hexane solution of 3 times the volume of the supernatant to the supernatant in step 2), d...

Embodiment 2

[0033] A method for detecting sparfloxacin enantiomers in aquatic products, comprising the following steps:

[0034] 1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%:10% as the mobile phase to dissolve and dilute sparfloxacin to a solution of 40 μg / mL, and filter with a microporous membrane;

[0035] 2) Take the homogenized aquatic product and place it in a centrifuge tube, add the sparfloxacin solution prepared in step 1), the solid-liquid ratio is 1g:120mL, add anhydrous copper sulfate and monoethanolamine after shaking, and centrifuge at 8000rpm for 10min , take the supernatant, the residue is dissolved with monoethanolamine and centrifuged, and the supernatant is combined for subsequent use; the addition of anhydrous copper sulfate is 3 times the quality of the aquatic product, and the addition of monoethanolamine is 1g of aquatic product and 20mL;

[0036] 3) Add a n-hexane solution twice the volume of the supernatant to the supernatant in step 2),...

Embodiment 3

[0040] A method for detecting sparfloxacin enantiomers in aquatic products, comprising the following steps:

[0041] 1) Use a mixture of isopropanol and n-heptane with a volume ratio of 90%:10% as the mobile phase to dissolve and dilute sparfloxacin to a solution of 45 μg / mL, and filter with a microporous membrane;

[0042] 2) Put the homogenized aquatic product into a centrifuge tube, add the sparfloxacin solution prepared in step 1), the ratio of solid to liquid is 1g:130mL, add anhydrous copper sulfate and monoethanolamine after shaking, and centrifuge at 9000rpm for 12min , take the supernatant, the residue is dissolved with monoethanolamine and centrifuged, and the supernatant is combined for subsequent use; the addition of anhydrous copper sulfate is 3 times the quality of the aquatic product, and the addition of monoethanolamine is 1g of aquatic product and 20mL;

[0043] 3) Add n-hexane solution of 3 times the volume of the supernatant to the supernatant in step 2), disc...

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Abstract

The invention relates to a method for detecting sparfloxacin enantiomer in an aquatic product. The solid-phase extraction conditions are optimized, so that the solid-phase extraction time is shortened, and the efficiency is high; besides, by means of the high performance liquid chromatography method, the concentration accuracy of sparfloxacin enantiomer is high, the speed is high, the operation is simple and the cost is lower; the detection method has good linear relation for a target compound, the recovery rate is high, relatively small deviation is caused, a used reagent is low-toxicity and small in dosage, and the method is environment-friendly.

Description

technical field [0001] The invention relates to a method for rapidly and efficiently detecting the enantiomer of sparfloxacin in aquatic products. Background technique [0002] Sparfloxacin has a good inhibitory effect on Gram-positive bacteria, Gram-negative bacteria, Mycoplasma, Chlamydia and Legionella. In addition, Sparfloxacin also has good absorption, low inhibitory concentration, and antibacterial activity High, not easy to produce drug-resistant bacteria, low toxicity and other advantages, has been used in aquaculture. [0003] At present, the commonly used separation methods of enantiomers of chiral drugs include crystallization, kinetic methods, enzymatic resolution and chromatography, etc. These methods are widely used and promote the research and development of chiral drugs. However, these methods also have some disadvantages, such as cumbersome crystallization, long separation time, and narrow applicability; enzymatic resolution has high requirements for enzyme...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14G01N2030/027G01N2030/146
Inventor 欧阳小琨金如娜杨立业王阳光王艳飞卢娇
Owner ZHEJIANG OCEAN UNIV
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