Method for detecting menbutone residues in porcine tissues
A technology of menbutone and tissue, applied in the field of analysis, can solve the problems of many side effects, small safety range, poor selectivity, etc., and achieve the effect of simple operation, high sensitivity and good accuracy
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Embodiment 1
[0031] Embodiment 1, the establishment of the residual detection method of monbutronone in porcine tissue
[0032] The method for detecting residues of menbutronone in porcine tissue, the specific steps are as follows:
[0033] (1) Pretreatment of tissue samples: Weigh 20 g of porcine tissue (muscle, fat, liver or kidney) after intramuscular injection of menbutrin injection, chop it up, and place it in a high-speed disperser (endo-type homogenizer), Homogenize at 6000r / min for 8min, then accurately weigh 2.0g of the homogenized tissue, add 4mL of acetonitrile, vortex mix, centrifuge at 3000r / min for 10min, take the supernatant, add acetonitrile repeatedly to extract 2 Combine the supernatants extracted three times, then transfer all the supernatants to a 50mL round-bottomed flask, and evaporate to dryness in vacuum at 60°C. The phase was ultrasonically dissolved and transferred to a centrifuge tube, and centrifuged at 10,000r / min for 10min, and the centrifuged supernatant was...
Embodiment 2
[0036] Embodiment 2, verification of tissue sample pretreatment method
[0037] (1) Homogenization speed
[0038] Take respectively 5 parts of pig's muscle (non-injection site and injection site), fat, liver and kidney after intramuscular injection of menbutronone injection, each part of about 20.0g, respectively at 2800, 4000, 5000, 6000, 7000r / Homogenize for 8 minutes under the condition of 1 min, and then operate according to the method of Example 1. Each tissue takes 2 parts of the test sample, and each part is continuously injected 2 times for analysis, and the reference substance solution is continuously injected 5 times. Calculated according to the external standard method. The average monbutronone content at the homogenization rotation speed, and calculate the relative deviation of the average monbutronone content between adjacent rotation speeds, the results are shown in Tables 1-5.
[0039] Table 1. Effects of different homogenization speeds on the determination of...
Embodiment 3
[0091] Embodiment 3, verification of the residual detection of menbutronone
[0092] The verification was carried out in accordance with the requirements of the Ministry of Agriculture document "Technical Specifications for Veterinary Drug Residue Testing (Trial)".
[0093] The specific chromatographic conditions are as follows: the chromatographic column is Shim-packVP-ODSC 18 Column (4.6×250mm, 5μm), octadecylsilane bonded silica gel as filler; mobile phase is acetonitrile and 0.5% phosphoric acid (55:45 by volume); column temperature is 25°C; detection wavelength is 235nm; flow rate The injection volume is 20 μL; the number of theoretical plates is not less than 2000 based on the monbutronone peak, and the separation degree between the monbutronone peak and the adjacent impurity peak is greater than 1.5.
[0094] Verification method: Accurately weigh 10 mg of menbutrin reference substance, dissolve it in acetonitrile and dilute to 100 mL, shake well, accurately measure 5.0...
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