Analysis method of monensin, salinomycin and lasalocid residues
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A detection method and drug technology, applied in the direction of analyzing materials, material separation, measuring devices, etc., to achieve the effect of improving sensitivity
Inactive Publication Date: 2013-12-04
HUAZHONG AGRI UNIV
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Domestically, there are reports on the methods for the total amount of monensin, salinomycin, methyl salinomycin and lasacelomycin residues in eggs, LC-MS/MS of monensin and s
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Embodiment 1
[0047] Embodiment 1: the derivatization reaction of carboxyl compound and bromoacetylpyrene
[0048] (1) Monensin sodium, salinomycin sodium, Lasalocid (Lasalocid A sodium salt) derivatization reaction with bromoacetylpyrene
[0049] Accurately weigh an appropriate amount of monensin sodium, salinomycin sodium, and 100 mg of the reference substance of lasalocid (lasalocid A sodium salt), dissolve it in methanol into a 10 mL volumetric flask, and prepare a 10 mg / mL standard respectively. stock solution. Accurately draw 1500 μL, 600 μL, and 400 μL of standard stock solutions of monensin sodium, salinomycin sodium, and lasalocid (Lasalocid A sodium salt) into 10 mL volumetric flasks, dilute to the mark with acetonitrile, and mix well That is, (concentration: 1.5mg / mL, 0.6mg / mL, 0.4mg / mL, respectively). Take 1mL from each volumetric flask, put it into a 10mL volumetric flask, and dilute to the mark with acetonitrile to obtain mixed standard working solutions with respective conc...
Embodiment 2
[0062] Embodiment 2: sample determination
[0063] (1) Processing of samples
[0064] The muscle, liver and kidney tissues of chicken and pig were selected as experimental samples, and the addition and recovery experiment of monensin, salinomycin and lasalocid 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. Each tissue was repeated for 5 days, and the average recovery rate was calculated.
[0065] Extraction: Accurately weigh (5±0.05) g of fresh or thawed sample and place it in a centrifuge tube, add 15 mL of isooctane, vortex for 2 min, centrifuge at 8000 r / min for 10 min, take out the ...
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Abstract
The invention belongs to the technical field of veterinary drug residue analysis and discloses a high performance liquid chromatogram pre-column derivatization reaction analysis method for a hydrogen substitution derivatization reaction of carboxyl compounds of polyetherionophores. Carboxyl groups contained in polyetherionophores react with a fluorescent reagent of 1-(bromoacetyl) pyrene, and the products have extremely-high fluorescence. The following reaction conditions are optimized: a 18-crown ether-6 solution is used as a phase transfer catalyst; a 1-(bromoacetyl) pyrene solution is used as a derivatization reagent; the reaction is conducted in a water bath at 30-70 DEG C for 150 min; after being cooled, the products are detected through a high performance liquid chromatograph. The excitation wavelengths of the derivatives are 360 nm; the derivatives have the highest fluorescence intensity when the emission wavelengths of the derivatives are 420 nm; the minimum detectable amount is 50 Mug/L; the derivatives show linear response to peak areas within the range of 200-1600 [mu]g/L; the result reproducibility is high; the variable coefficient of 3 concentrations and 15 repetitions is smaller than 7.8%; all indexes can meet the residue analysis requirements of the three polyetherionophores of monensin, salinomycin and lasalocid.
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 a rapid detection method and application of polyether drugs monensin, salinomycin and lasaloxil residues. In the present invention, polyether drug 18-crown-6 solution is used as a phase transfer catalyst, 1-bromoacetylpyrene solution is used as a derivatization reagent, and a derivatization reaction system is constructed with carboxyl-containing polyether drugs to obtain a test standard sample, and then passed High performance liquid chromatography for separation and detection. Background technique [0002] Polyether antibiotics are also called polyether ionophores (Polyetherionophores). Such drugs have antibacterial and anti-coccidian effects, and can promote animal growth and development and improve feed conversion rate, etc. Drugs in this class mainly include monensin, salinomycin, and lasa...
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