This standard specifies the determination method of chloramphenicol in livestock and poultry meat. This standard is applicable to the inspection of chloramphenicol in livestock and poultry meat. SB/T 10386-2004 Determination of chloramphenicol in livestock and poultry meat SB/T10386-2004 Standard download decompression password: www.bzxz.net

ICS 67.120
Registration No.: 14167—2604
Domestic Trade Industry Standard of the People's Republic of China SB/T10386—2004
Determination of chloramphenicol in meat of livestock and poultry
Determination of chloramphenicol in meat of livestock and poultry
Promulgated on August 4, 2004
Ministry of Commerce of the People's Republic of China
Implementation on September 1, 2004
This standard is issued by the Ministry of Commerce of the People's Republic of China
SB/T10386—2004
This standard was drafted by the Technical Standardization Center of the Ministry of Commerce, the Nutrition and Food Safety Institute of China National Center for Disease Control and Prevention, and the Hebei Provincial Center for Disease Control and Prevention.
The main drafters of this standard are: Liu Wenqi, Yang Zuying, Shu Shi, Han Huixin, Zhang Xinzhong, Liu Hucheng. The Ministry of Commerce Technical Supervision Center is responsible for the interpretation. 1 Scope
Determination of chlorinated substances in livestock and poultry meat
This standard specifies the method for the determination of chlorinated substances in cooked meat. This standard is applicable to the test of chlorinated substances in cooked meat and high-quality meat. 2 Principle
SB/T 10386—2004
The residual chlorinated substances in the sample are extracted with ethyl acetate, concentrated under reduced pressure, and decomposed with C.5mol/1 ... 3. Reagents and Materials
The following reagents are all analytical reagents except those specified in the following sections. 3.1 Water is deionized water, not alcohol, chromatographic absolute.
3.2 Standard,
3.3 Chloride is equivalent to 491 units per mg, content 99%. 3.4 Ethyl
3.5 High temperature acid
3.6 Cyclopentanone standard stock solution: Accurately weigh C.010g of chloramphenicol standard solution and put it into a 100mL volumetric bottle. Use two solutions and dilute to full scale, and adjust. The viscosity of this solution is G, 1mR/mT. Store in a refrigerator: valid for 3 months. 3.7 Oxygen should be used in a standard working cup, and the sample is 5.0mL of stock solution minus 50mL. Put it into a narrow volumetric bottle and add medium alcohol to the mark. The concentration of this solution is 10/mL. Store in ice, valid for half a year. Before use, dilute this solution with 0.5/L sodium bicarbonate to a suitable concentration. 1. Heat the mixture.
4 Instruments and equipment
4.1 High-performance liquid chromatograph (with external detector). 4.2 Heat the mixture.
4.3 Cooling evaporator.
4.4 Addition of energy
4.5 Rotary evaporator. Www.bzxZ.net
4.5 Micro-membrane filtration.
5 Determination steps
5.1 Extraction
Take 290 μg of the sample, take 20 μg (accurate to 0.01 g), crush the sample, place it in a 100 μl triangular tube, and add 10 μl. 1.0ml 0.3mol/1.5mol/l high-efficiency washing agent was added to the bottle, and 1ml n-hexane was added. After 1min of shaking, the whole solution was extracted with 2% ethyl acetate in a vacuum flask, and then ultrasonically extracted with 1:10 ml ethyl acetate. The mixture was separated, and then ultrasonically extracted with 2% ethyl acetate for 15min. After 1min of shaking, the mixture was combined and transferred to a new bottle.
5.2 Purification
The combined solution was concentrated to dryness in 52°C~5F water in an evaporator. Add 1.0ml 0.3mol/1.5mol/l high-efficiency washing agent to the bottle, add 1ml n-hexane, shake for 1min, transfer the whole solution to a 50L test tube, stop stratification, 1
S3,T103—2C04
Aspirate the second layer, and then add? .1 alkane lock fat side and then absorb the n-dioxane layer, produce chlorine magnetic flux through 0.4Sm frequency connection, end liquid for high performance liquid chromatography determination.
5.3 Bay determination
dropwise phase chromatography full meal test conditions
E) Spectroscopy.IypersicDs22cmmm4,5mw particle diameterEptt; mobile phase: back-water 45+55
c flow rate: 1.cmLinin
d) Detection wave, 2xonm:
t! Column: Implementation:
) Injection volume: 2n pl.,
5.3.2 Preparation of standard solution
According to the above chromatographic conditions, inject the standard working solution into each point, and measure the peak area of ​​each standard solution. Then, make a grid with the standard limit thickness against the source area, and calculate the autoregression equation and correlation coefficient. 5.3.3 Preparation of sample
Under the above chromatographic conditions, take 20)L of the purified sample solution for HILC analysis. 6 Results
6.1 Calculation
Carry out regression analysis on the concentration of each point of the standard solution and the corresponding concentration, and then calculate the content of chlorine in the sample according to the formula>.
In the formula:
#×00g
Content of the sample, in nominal grams per gram (mg/kg); Content of the test solution, in micrograms per liter (μg/liter); Volume of the sample, in actual volume (μg/liter);
Mass of the sample, in grams (e).
E.2 Limit of detection
The detection limit of this sequence is c.3:\R/al. When the detection limit is 2)g, the minimum detection limit is 1.cg/kg:? Allowable error
The difference between two consecutive determination results of the same analysis shall not exceed 15% of the mean value.
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