Pirlimycin residue analysis method

A technique for analysis of pyrithycin and residues, which is applied in the field of analysis of residues of pyrithycin to achieve the effects of high ultraviolet absorption intensity, high fluorescence activity, and fast reaction speed

Inactive Publication Date: 2013-12-04
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no high performance liquid chromatography residue detection method

Method used

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  • Pirlimycin residue analysis method
  • Pirlimycin residue analysis method
  • Pirlimycin residue analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1: Derivatization reaction of secondary amino compound with 9-fluorenylmethyl chloroformate

[0042] (1) Derivatization reaction of pyrithycin and bromoacetylpyrene

[0043] Accurately weigh 10 mg of the reference substance of pyrithycin, dissolve it into a 10 mL volumetric flask with methanol, and prepare 1 mg / mL standard stock solution respectively. Accurately pipette an appropriate amount of standard working solution, and dilute it successively with methanol to concentrations of 5 μg / L, 10 μg / L, 20 μg / L, 50 μg / L, 100 μg / L, 200 μg / L, 500 μg / L, 1000 μg / L, 2000 μg / L L standard working solution. Accurately pipette 40 μL of standard working solution, add 80 μL of boric acid buffer in sequence (configuration method: accurately measure 0.38 g of sodium tetraborate, dissolve and dilute with water, adjust pH=9.0 with hydrochloric acid, and dilute to 100 mL volumetric flask) and 80 μL of derivatization Reagent (accurately weigh 26mg of 9-fluorenylmethyl chloroformate...

Embodiment 2

[0050] Embodiment 2: sample determination

[0051](1) Processing of samples

[0052] The bovine muscle, milk and bovine kidney were selected as the experimental samples, and the addition and recovery experiment of pilinomycin was carried out. Add an appropriate amount of standard solution to the blank sample, so that the concentration in the sample is LOQ, 1MRL, and 2MRL respectively (the specific concentration of each drug is shown in the table below), and the sample is tested after pretreatment. Repeat 5 samples for each concentration on the same day, calculate the recovery rate, and take the average value to calculate the intra-day coefficient of variation; repeat 5 days for each tissue, and calculate the average recovery rate.

[0053] Extraction: Accurately weigh 5g of fresh milk or thawed beef muscle and kidney samples and place them in a centrifuge tube, add 10mL of 1% formic acid acetonitrile, vortex and mix for 1min, centrifuge at 8000r / min for 10min, take out the su...

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Abstract

The invention belongs to the field of veterinary drug residue analysis and relates to a pirlimycin residue analysis method. According to the invention, a high-performance liquid chromatograph pre-column derivatization reaction analysis is adopted for a hydrogen substitution reaction of a secondary amine compound. At the room temperature, the concentration of a derivatization reagent, chloroformic acid-9-fluorenylmethyl ester, is 10-2 mol/L, a pH value of a borate buffer solution of 0.1 mol/L is regulated to 9, the reaction is an instant reaction, as only one secondary amine is used as a single reaction site, no reaction terminator is required to be added to achieve the purpose of derivatization, and the derivation product is stable. The derivation product is subject to high performance liquid chromatograph detection, has the maximum ultraviolet strength when the ultraviolet detection wavelength is 266 nm, has the minimum detectable amount of 5 mug/L, is in linear response to the peak area within the range of 20-4000 [mu]g/L, is good in reproducibility of results, and has three concentrations, and the variable coefficient of 3 concentrations and 15 repetitions is smaller than 8%.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug residue analysis and is related to analytical chemistry. The invention specifically relates to an analysis method for the residue of the marked compound pilimycin. The invention uses 9-fluorenylmethyl chloroformate as a derivative reagent The residual level of the marked compound pilinomycin in the animal products to be tested is determined by the pre-column derivatization method and the HPLC method for joint measurement with the pilinomycin drug containing a secondary amino group. Background technique [0002] Pilithromycin is a veterinary antibiotic drug, insoluble in water, its hydrochloride is soluble in methanol and propylene glycol, and slightly soluble in water. Hydrochloride contains 1 crystal water, is white or off-white powder, molecular formula is C 17 h 31 ClN 2 o 5 S·HCl·H 2 O, molecular weight 465.43, chemical name (2S-cis)-methyl 7-chloro-6,7,8-trideoxy-6-[[(4-ethyl-2-p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 袁宗辉陶燕飞陈冬梅潘源虎王玉莲黄玲利王旭刘振利谢书宇彭大鹏戴梦红郝海红程古月
Owner HUAZHONG AGRI UNIV
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