This standard specifies the method for determining the content of nicarbazin in feed by high performance liquid chromatography. This standard is applicable to the determination of nicarbazin in compound feed, concentrated feed and premixed feed. The minimum detection concentration of this method is 1 mg or more of nicarbazin per kilogram of feed. GB/T 19423-2003 Determination of nicarbazin in feed by high performance liquid chromatography GB/T19423-2003 Standard download decompression password: www.bzxz.net
This standard specifies the method for determining the content of nicarbazin in feed by high performance liquid chromatography. This standard is applicable to the determination of nicarbazin in compound feed, concentrated feed and premixed feed. The minimum detection concentration of this method is 1 mg or more of nicarbazin per kilogram of feed.

ICS65.120
National Standard of the People's Republic of China
An B/T19423—2003
Determination of nicarbazin in feed-High performance liquid chromatography
Determinatiou of nicarbazin in feed-High performance liquid chromatography chromntograph2003-12-11 Issued
People's Republic of China
General Administration of Quality Supervision, Inspection and Quarantine
2004-06-01 Implementation
GB/T19423-2003
This standard test method is mainly based on the "Test Method of Nitrate in Feed" in Section 3 of the American Standard Drug Analysis Card for the Identification of Defective Drugs (TDA) in Animal Tissue Dissociation. It is determined through experiments. The standard was proposed by the National Standardization Technical Committee of the State Administration of Industry and Information Technology of the State Council. This standard was made under the jurisdiction of the National Technical Committee for Standardization of the National Standardization Technical Committee of the National Standardization Technical Committee of the State Council. The drafting unit of this standard The main contributors to this standard are: Mo Congmei, Yi Shirong, Bu Qingshang, Lu Xingjiang, Bi Benfang and Zhang Zhikai. t
Determination of Nicardin in Feed
High Performance Liquid Chromatography
This standard specifies the method for determining the content of nicardin in feed by using a commercial liquid chromatography instrument. This standard is applicable to the determination of nicardin in combined feed, concentrate feed and/or mixed feed. The minimum detection concentration of this method is 1mR or more per kilogram of feed: 2 Normative references
GB/T19423—2003
The clauses in the following documents become the clauses of this standard through the application of this standard. , it is the referenced document of Jiangkou Yu. Its subsequent amendments (excluding the incorrect internal insertion) are not applicable to this standard: but the parties to the analysis agreement reached according to this standard may use the later versions of these documents. For any incorrect referenced document, its revised version shall apply to this standard. GB/T6692-1002 Analysis of the age of the case using hydrothermal format and test method 3 Principle
DM is extracted from the sample by hydrothermal chromatography. It is purified by oxidation chromatography, concentrated and eluted with a solution, determined by commercial chromatography, C. and phase, with methyl methacrylate as the precipitant, and a UV detector with a wavelength of 56 Quantitative determination was carried out under the condition of 5nm.
4 Equipment
4.1 High performance liquid chromatography with external detector. 4.2 Chromatographic instrument: cm reaction cabinet (particle size 5m, inner diameter 0cm, length 0cm, inner diameter 1.6mm) 4.3 Rotating generator.
4.4 Electric belt drive
4-layer nuclear tube:
5 Reagents and solutions
The following reagents and water are analytical grade unless otherwise specified. Water is of the scientific grade specified in (13/DIN 6682-1992).
5.2 Chromatographic purity,
5.3 Dimethylformamide (DMF).
5.4 Alkaline oxidizing agent: 100-200 days, 105 pieces of record, dry for 2h, then put into the olefin reactor, 5.5 elution, 55% 2-alcohol (.1) aldehyde (5.2 is 915.5. Nicarbamide solution: accurately weigh 1mm Nicarbamide standard, make up to 1Ccml with DMF (concentration is 1g/L). 5.7 Nicarbamide solution, 1mL Nicarbamide solution (5.) quantify with TMF to 10 0l (concentration is 1J\g/L).5.8 Mobile phase, 83+20% methanol solution.6 Sample preparation
Select representative samples and additives, crush to 500 g, grind to 0.45mm pore size analysis sieve, filter spoon, sealed container.
7 Analytical procedure
7.1 Sample preparation
7.1.1 Extraction
Use a 20% ionizer with a 50mV electrophoretic separator (1MF) according to 3V, filter through grade 1, collect the residue, and prepare 7.1.2 Column chromatography purification
7.1.2. 1. Preparation of column
Add about 2/3 tube height of dimethylformamide (1MF) to the mass spectrometer and slowly add the oxidizing agent to the highest standard of about 6rm, carefully remove bubbles, let it stand for 15, and then add the active agent until the liquid reaches the surface of the alumina. Then add 2r.T>MF to wash the column. Note that the liquid level cannot be lower than the surface of the oxidizing agent.
7.1.2.2 Purification
Accurately transfer 23ml of the chromatographic column, add the liquid until the liquid level reaches the surface of alumina, elute the column with 25mDMF, discard the eluent, elute the nicotinic acid immediately, and vigorously add the first 1~3 eluents. If the nicotinic acid does not flow out during the above process, collect the remaining eluent and transfer it to the incubator flask. Evaporate it with a rotary incubator at 607C to 10, use up the eluent and stop the last recording. The concentration is 1u/m1. If other diameter chromatographic tubes are used for analysis, the inner diameter of the chromatographic tube should be changed by 7.2. The concentration of Nicarbamide standard solution is 1u/m1. If other diameter chromatographic tubes are used for analysis, the inner diameter of the chromatographic tube should be changed by 7.2. 7.1.2: Prepare Nicarbamide working solution. Transfer 25mL of Nicarbamide working solution to the standard pound. Follow the steps in 7.1.2.3 until the “Note” is reached. Collect the missing liquid in a 2mL volumetric flask. Use eluent to make up to the scale, 7.3 Adjust
7.3.1 High efficiency reverse phase chromatograph
7.3.1.1 Chromatographic column: C reverse phase (particle size 5m, inner diameter 4.6cm, length 10cm) 7.3.1.2 Flow or phase precipitation 1 water 80120)
7.3.1.3 Flow: 1nL/mir.
7.3.1.4 Warm slowly, temperature.
,3.1.5 Input volume: 1 nm..
7.3.1. Detector: external detector. Wavelength 365 nm..7.3,2 Determination on the machine
Carbazine standard drop and test solution are injected into the chromatograph respectively, and the colorimetric graph is recorded. The result is calculated by external recognition.7,4 Calculation and expression of results
7.4.1 Calculation formula
Continue the calculation formula (1: Calculation formula:
C-PxGixV?
C一: The content of carbazine in the test solution is in grams per gram (mg/g); the content of carbazine in the standard solution is in micrograms per gram (e/ml. Test peak area response value:
1 Standard solution peak response value:
Test solution volume, unit is liter (rL): mbZxz.net
Sample mass, unit is g);
2 Test dilution factor,
.4.2 Parallel determination results are shown using the arithmetic half-mean, retaining one significant figure and allowing integers to be
CB/119423—2003
The same analyst shall determine (or re-determine) the same sample at the same time and obtain a new result: The deviation of the test solution content above 1 mg/kg is not more than %, and the confidence interval above 10 mg/kg is not more than 1%.
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