Determination method for β-lactam antibiotic residues in milk
A technology of lactams and detection methods, which is applied in the direction of analyzing materials through chemical reactions and observing the impact on chemical indicators, etc. It can solve the problems of cumbersome operation steps, long detection time, poor selectivity, etc. problem, to achieve the effect of simple operation method, fast detection speed and high accuracy
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Embodiment 1
[0021] 1. 100 milliliters of antibiotic-free milk (blank) samples and 100 milliliters of milk samples to be tested are mixed with 50 milliliters of acidified acetonitrile respectively, and then centrifuged at 3000 r / min for 3 min. Said acidified acetonitrile is composed of hydrochloric acid: acetonitrile by volume = 1:1 prepared;
[0022] 2. Then use 1% dilute sulfuric acid to adjust the pH value of the centrifuged sample supernatant to 6, add 0.1g / L copper sulfate solution according to the volume ratio of the supernatant to 1:2, shake well and let it stand for 15 minutes to react;
[0023] 3. Use a UV spectrophotometer to test the UV absorbance value of the supernatant after the reaction at 240nm, record and compare the data to determine whether there are β-lactam antibiotics left in the milk sample to be tested. Record the data and calculate that the content of β-lactam antibiotics in the blank sample is 0.01mg / L, the content of β-lactam antibiotics in the sample to be teste...
Embodiment 2
[0025] 1. 100 milliliters of antibiotic-free milk (blank) samples and 100 milliliters of milk samples to be tested were mixed with 200 milliliters of acidified acetonitrile respectively, and then centrifuged at 800 r / min for 10 min. Said acidified acetonitrile was composed of hydrochloric acid: acetonitrile by volume ratio = 1:2 prepared;
[0026] 2. Then use 10% dilute sulfuric acid to adjust the pH value of the centrifuged sample supernatant to 2, add 2g / L lead acetate solution according to the volume ratio of the supernatant to 1:2, shake well, and let it stand for 5 minutes;
[0027] 3. Use a UV spectrophotometer to test the UV absorbance value of the supernatant after the reaction at 380nm, record and compare the data to determine whether there are β-lactam antibiotics left in the milk sample to be tested.
[0028] Record the data and calculate that the blank sample β-lactam antibiotic content is 0.85mg / L, the test sample β-lactam antibiotic content is 1.04mg / L, and the y...
Embodiment 3
[0030] 1, 100 milliliters of antibiotic-free milk (blank) samples and 100 milliliters of milk samples to be tested were mixed with 100 milliliters of acidified acetonitrile respectively, and then centrifuged at 1500 r / min for 8 min. Said acidified acetonitrile was composed of hydrochloric acid: acetonitrile by volume ratio = 1:5 prepared;
[0031] 2. Use 6% dilute sulfuric acid to adjust the pH value of the supernatant of the centrifuged sample to 3, add 1g / L cobalt chloride solution according to the volume ratio of the supernatant to 1:2, shake well, and let it stand for 8 minutes;
[0032] 3. Use a UV spectrophotometer to test the UV absorbance value of the supernatant after the reaction at 320nm, record and compare the data to determine whether there are β-lactam antibiotics left in the milk sample to be tested.
[0033] Record the data and calculate that the blank sample β-lactam antibiotic content is 0.93mg / L, the test sample β-lactam antibiotic content is 1.21mg / L, and t...
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