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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

Inactive Publication Date: 2010-07-14
云南健牛环境监测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned methods have their own strengths in detection precision, etc. Some have low sensitivity and poor selectivity; Processing enterprises cause a lot of inconvenience

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention discloses a method for measuring the amount of residual penicillin in milk. Standard working anhydrous alcohol solution with penicillin sodium is prepared, the pH value is regulated by dilute HCl to 2 plus or minus 0.5 or 4 plus or minus 0.5, the standard working anhydrous alcohol solution is bathed in boiling water, so that degradation products, i.e. penicillamine and penicillenic acid, are obtained, then the two degradation products respectively react with benzoquinone substance, so that charge-transfer complexes are obtained, and the working curves of different charge-transfer complexes are calculated. During measurement, the absorbance of the charge-transfer complex of milk sample is calculated by the same way, and is substituted into the working curve of the charge-transfer complex to work out the amount of the residual penicillin in the milk. The invention takes the lead in directly using the ultraviolet or fluorescent spectrophotometry to measure the amount of the residual penicillin in the milk. The method has the advantages of quick measurement, wide measurement range, high sensitivity, high accuracy and good selectivity, an expensive antibiotic detection instrument does not need to be purchased, the operation method is simple, and the method can reduce the production cost and the operation risk for diary processing enterprises, and therefore having a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and relates to a method for detecting residual antibiotics in milk, in particular to a method for detecting residual penicillin in milk. Background technique [0002] In industrial dairy farming, antibiotics are often used to treat bovine mastitis and other cow diseases, and these antibiotics are inevitably transferred to the milk in the first few days. Antibiotic residues in milk can seriously affect the quality of dairy products. The food laws of the World Food and Agriculture Organization (FAO) and the World Health Organization (WHO) have clear regulations on the maximum residue limit of antibiotics in milk, and the European Union has also made detailed regulations on the maximum residue level (MRL). In 2001, the Ministry of Agriculture of my country promulgated and implemented the "Non-Pollution Food Raw Milk Industry Standard", which clarified the hygienic indicators of fresh ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N21/64G01N1/28G01N1/44
Inventor 杨亚玲耿卫东
Owner 云南健牛环境监测有限公司
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