A method for the quantitative detection of fluoroquinolones in chicken manure
A technology for quantitative detection of fluoroquinolones, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low recovery rate of analysis and determination technology, difficult analysis and determination of FQs, high cost, etc., and achieve the effect of low analysis cost
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Embodiment 1
[0036] Compared with 50% Mg(NO 3 ) 2 -2.5% NH 3 ·H 2 O, EDTA-Mcllvaine buffer (pH=4) and acetonitrile and other inorganic and organic extracts, methanol: acetic acid: water (6:1:3, V / V) and EDTA-Mcllvaine: acetonitrile (1:1, V / V) V) and other mixed extracts, and EDTA-Mcllvaine buffer and methanol: acetic acid: water (6:1:3, V / V) recovery rate of each target compound extraction. The results are shown in Table 1. It can be seen from the table that the use of the inorganic extract 50% Mg(NO 3 ) 2 -2.5% NH 3 •H 2 O, EDTA-Mcllvaine buffer or organic extract acetonitrile, all can not effectively extract the target from the matrix; while using organic-inorganic mixed extract methanol: acetic acid: water (6:1:3, V / V), The extraction efficiency of target substances such as NOR and CIP is still low. When using EDTA-Mcllvaine buffer solution and methanol: water: acetic acid = 6:1:3 for compound extraction, the extraction efficiency can basically meet the requirements, but the amou...
Embodiment 2
[0044] Choose EDTA-Mcllvaine: acetonitrile (1:1) as the extractant, adjust the pH of the extract to 1.0-8.0 with HCL or NaOH, extract the sample, pass through the SPE column and measure it on the machine, and study the pH value of the extract extraction efficiency. The results are shown in Table 2. The recovery rate of each target substance is significantly affected by the pH change of the extractant. Within a certain range, the recovery rate of antibiotics increases with the decrease of pH. When pH ≥ 5, the recovery rate of the target substance is low, less than 60%, and when the pH ≤ 3.0, the recovery rate of the six fluoroquinolones is higher, above 68.5%, and the recovery rate is the best at pH = 2 , up to 76.6% to 104.3%, and the impurities contained in the extract are relatively small. Therefore, EDTA-Mcllvaine: acetonitrile = 1:1 was selected as the extractant, and the extraction efficiency was the best when the pH value was adjusted to 2.
[0045] Table 2 Comparison ...
Embodiment 3
[0048] An example of the invention is listed below, and the present invention is further described in conjunction with data, but the present invention is not limited to this example.
[0049] Chicken manure samples came from 4 large-scale chicken farms in the suburbs of Beijing (chicken farm 1, chicken farm 2, chicken farm 3 and chicken farm 4) and 1 natural free range farm (chicken farm 5, the chicken farm Antibiotics such as FQs have not been used in the field). Use a stainless steel shovel to collect fresh chicken manure on the same day in the chicken house of the chicken farm, collect and mix it at multiple points in a chicken farm to form a chicken manure sample, and seal it away from light (each chicken farm sample is numbered No. 1, 2 in sequence) No. 3, No. 4, No. 5), brought back to the laboratory and stored at -10°C. Take an appropriate amount from the chicken manure sample, freeze-dry, crush and pass through a 2mm sieve, take 0.5±0.005g of ground and sieved sample ...
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