Method for measuring amount of residual penicillin in milk
A technology for penicillin and residual content, which is applied in the preparation of test samples, measurement of color/spectral characteristics, fluorescence/phosphorescence, etc. It can solve the problems of cumbersome operation steps, long detection time, poor selectivity, etc., and achieve simple operation methods , Fast detection speed and high accuracy
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Embodiment 1
[0022] The milk samples in the following examples are fresh milk purchased by milk production enterprises.
[0023] 1. Take 100mL, 0.50mg / L penicillin sodium standard working absolute ethanol solution in a small beaker. Adjust the pH to 4 with dilute HCl, bathe in boiling water for 10 minutes, and degrade to obtain penicramic acid.
[0024] 2. Take 3 mL of penicillin acid, the degradation product of penicillin sodium, in a 10 mL colorimetric tube, add 3.00 mL of 5×10 -3 mol / L chloranil anhydrous ethanol solution, dilute to the mark with ethanol, shake well, and stand at room temperature for 10 min to obtain the charge-transfer complex.
[0025] 3. The above charge-transfer complex solution was used to measure the fluorescence intensity of the charge-transfer reaction product with 323nm as the excitation wavelength and 475nm as the emission wavelength, and a blank test was performed at the same time.
[0026] 4. Take 1mL, 5mL, 10mL, 20mL, 30mL of the degraded penicillin solut...
Embodiment 2
[0031] 1. Take 100mL, 0.50mg / L penicillin sodium standard working absolute ethanol solution in a small beaker. Adjust the pH to 2 with dilute HCl, bathe in boiling water for 20 minutes, and degrade to obtain penicillamine.
[0032] 2. Take 3 mL of penicillamine, the degradation product of penicillin sodium, in a 10 mL colorimetric tube, add 5.00 mL of 1×10 -3 mol / L chlorobenzoquinone absolute ethanol solution, dilute to the mark with ethanol, shake well, and stand at room temperature for 5 minutes to obtain a charge-transfer complex.
[0033] 3. Use the above charge-transfer complex solution to measure the ultraviolet intensity of the charge-transfer reaction product with 400nm as the ultraviolet absorption wavelength, and do a blank test at the same time.
[0034] 4. Take the degraded penicillin solution 1mL, 5mL, 10mL, 20mL, 30mL in step 1, and carry out the charge transfer ultraviolet measurement according to the steps 2 and 3. The linear regression equation is A=0.03901C+...
Embodiment 3
[0037] 1. Same as Example 1.
[0038] 2. Take the above 3mL penicillin sodium degradation product in a 10mL colorimetric tube, add 3.00mL 5×10 -3 mol / L p-benzoquinone acetone solution, dilute to the mark with acetone, shake well, and place at room temperature for 10 minutes.
[0039] 3. Using the above solution as the excitation wavelength of 335nm and the emission wavelength of 460nm to measure the fluorescence intensity of the charge transfer reaction product, and do a blank test at the same time.
[0040] 4. Take 1mL, 5mL, 10mL, 20mL, 30mL of the degraded penicillin solution in step 1, and perform charge transfer fluorescence measurement according to steps 2 and 3. The linear regression equation is A=0.06412C+0.07634, and the linear range is 0.1mg / L- 50mg / L, correlation coefficient r=0.9992, recovery rate 97%-103%, relative standard deviation 2.8% (n=6), detection limit 0.1mg / L.
[0041] 5. Take 100mL of milk samples containing penicillin sodium antibiotics and 5g of sodium...
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