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Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton

A sulfonamide drug and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of cumbersome steps and high cost, and achieve the effects of less consumption of organic solvents, shorter time consumption, and less pollution

Inactive Publication Date: 2016-01-20
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the shortcomings and deficiencies such as high cost and cumbersome steps of the sulfa antibiotic detection method in the above-mentioned prior art, the object of the present invention is to provide a detection method for 18 kinds of sulfa antibiotics in beef and mutton

Method used

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  • Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton
  • Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton
  • Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Weigh 5.00g (accurate to 0.01g) of homogeneous beef muscle tissue sample and add 6.00g anhydrous MgSO to 50mL 4 1.5g sodium acetate polypropylene centrifuge tube, accurately add 20mL 2% acetic acid-acetonitrile solution, homogenize at 18000r / min for 2min with a homogenizer, centrifuge at 4000r / min for 5min, take the supernatant to be purified.

[0033]Take 10mL of the supernatant and put it in a 15mL centrifuge tube, add 750mgMgSO 4 , 160mgPSA, 100mgGCB and 50mgC 18 , vortex the centrifuge tube vigorously for 2 minutes, centrifuge at 4000r / min for 5 minutes, take 5 mL of the supernatant, blow it to nearly dry with nitrogen, dissolve it with 1 mL of 20% methanol aqueous solution to 1 mL, pass it through a 0.22 μm filter membrane, and wait for determination.

[0034] Chromatographic conditions

[0035] Liquid chromatograph: Waters1525 high performance liquid chromatograph (with 2475 fluorescence detector);

[0036] Column: Dikma Platisil ODSC i8 4.6mm×250mm, the fille...

Embodiment 2

[0052] Weigh 5.00g (accurate to 0.01g) of homogeneous mutton muscle tissue sample and add 5.00g anhydrous MgSO to 50mL 4 , 2.5g sodium acetate polypropylene centrifuge tube, accurately add 20mL of 1.5% acetic acid-acetonitrile solution, use a homogenizer to homogenize at 15000r / min for 2min, centrifuge at 4000r / min for 5min, and take the supernatant to be purified.

[0053] Take 10mL of the supernatant and put it in a 15mL centrifuge tube, add 500mgMgSO 4 , 100mgPSA, 200mgGCB and 50mg neutral multi-walled carbon nanotubes, vortex the centrifuge tube for 2min, centrifuge at 4000r / min for 8min, take 5mL of the supernatant, blow it to nearly dry with nitrogen, and dissolve it with 1mL of 15% methanol aqueous solution to 1mL , through a 0.22μm filter membrane, to be determined.

[0054] Chromatographic conditions

[0055] Liquid chromatograph: Waters2965 high performance liquid chromatograph (with 2475 fluorescence detector).

[0056] Column: KromosilODSC 18 4.6mm×250mm, the f...

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Abstract

The invention discloses a method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton. The method comprises taking 5g of uniform beef and mutton, adding anhydrous magnesium sulfate, sodium acetate and acetonitrile acetate solutions into the beef and mutton, carrying out high-speed homogenized extraction, carrying out centrifugation, carrying out vortex mixing purification impurity-removal on the supernatant by an adsorbent containing a plurality of purification materials, carrying out pressure reduction or nitrogen blowing condensation on the supernatant subjected to re-centrifugation until drying, redissolving the residues, after shaking-up, filtering the solution by a microfiltration membrane with pore sizes of 0.22 micrometers to obtain a sample solution, carrying out separation by a reversed phase column filled with C18 as a filler, carrying out ultraviolet light on-line rapid derivation, carrying out detection by a fluorescence detector, carrying out qualitative analysis according chromatographic peak retention time, carrying out quantification by an external standard method and calculating residual quantity of 18 sulfanilamide drugs in beef and mutton. The method has simple processes, utilizes less amount of a reagent, has high detection sensitivity, releases simultaneous rapid detection of 18 sulfanilamide drugs by one step, greatly shortens analysis time and has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of food safety detection, in particular to a detection method for 18 kinds of sulfonamide antibiotic residues in muscle tissue of cattle or sheep. Background technique [0002] Beef and mutton are meat products with large consumption. They are rich in nutrients, rich in protein, fat, phospholipids, multivitamins, minerals and calcium, phosphorus, iron, zinc, copper, manganese and other trace elements. Beef and mutton have high nutritional value, are an important source of human nutrition, and are also a large amount of meat consumption. [0003] Sulfonamides are synthetic antibiotics with the structure of p-aminobenzenesulfonamide. They are widely used in animal husbandry because of their wide antibacterial spectrum, low price and convenient use. However, excessive use of sulfonamides will accumulate in animals such as cattle and sheep, and accumulate in the human body through foods such as beef and mutton,...

Claims

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Application Information

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IPC IPC(8): G01N30/06
Inventor 肖远灿胡风祖许旭董琦迟晓峰谭亮耿丹丹
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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