Some standard content:
c8 67.040
National Standard of the People's Republic of China
GB/T5009.87—2003
Substituted for B/T248—16C. Partially recommended for GB1310] [SS] Determination of phosphorus in foods
Determinatlon of phosphorus in foods2003-08-11PromulgatedbzxZ.net
Ministry of Health of the People's Republic of China
China National Standards Administration
2004-01-01Implementation
GB/T 5009.B7-2003
This standard corresponds to IS3946 Determination of total estrogen in starch and starch products (182 edition) and IS394621 Determination of total estrogen in milk and milk products - Molecular absorption method (1938 edition): This standard is consistent with IS394 and IS39462, but is not equivalent. This standard replaces the method for determination of total estrogen in foods and 1 3101159 Pi steaming period Huihuo standard 6.2 phosphate delimitation,
Compared with T1-, this standard is modified as follows:
Modified the Chinese name of the standard, the Chinese name of the standard is H20C1, 1-\ standard writing part 4: chemical analysis of the structure of the bottom standard.
GB13211991 four-style dyeing and boiling, all need ham stop The determination of 36.2% of the phosphine in human food is changed to the second method for the determination of phosphonates in food:
This standard is proposed by the Ministry of Health of the People's Republic of China. The first method is the first method, and the second method is the research institute of nutrition and food health of the Chinese Academy of Sciences, the Beijing Institute of Health is responsible for the labor; the first food hygiene inspection and testing institute of Xinhai, Shandong Province, and the Jiangxi Province Food Hygiene Supervision and Inspection Institute.
The main drafters of the first and second methods of this standard are: Tu Guangye, Shanning, Tu Xiaoming, Men Shihua; the main drafters of the second method are: Zi Peizhen, Yanli, Pu Zhai, Zheng Li, and Bu Qianzhan.
The original standard was issued in 1590. This time it is the second revision. Gsu
1 Scope
Determination of phosphorus in food
This standard stipulates the "spectrophotometric method for the determination of phosphorus in food: G0/T ECG3.87--2003
This standard, the first method is applicable to the determination of total phosphorus in food, the third method is applicable to the determination of complex acid salts and phosphates in Calcium carbonate, chlorinated acid and chlorinated acid.
The detection limit of the first method is ? 550, the molecular weight of the first method is 10.
The first method is spectrophotometric method
2 Principle
The organic matter in food is acidified and then reacts with ammonium sulphate under certain conditions to produce ammonium phosphate. This compound reacts with 2-hydroxy-2-nitropropene to form a blue compound. The absorption value of the spectrophotometer is measured at a wavelength of nm to analyze the sugar content.
3 Reagents
3.1 Sulfur: Sample preparation].81.
3,2-chloro-2-aldehyde is a mixture of chlorinated aldehydes. 3.315 Take 51% of the acid solution and dilute it with cold water. 3.4 Ammonium hydroxide solution: weigh 1N MoO4HO and dilute it to 1CCmL with 15% sulfuric acid. 3.5 Prepare the second solution: weigh 0.5% of the solution in 10mL of water and dissolve it. 3. White sulfonic acid solution: weigh 2% anhydrous sulfoxide in 100ml of water and dissolve it. Note: The solution needs to be prepared temporarily before the experiment: If it is tested, the blue solution may cause dust.
3.7 Phosphorus standard solution <100ug/ml.), weigh 115 μl potassium dihydrogen phosphate <0.44 μl in a 200 μl volumetric medium, add water to decompose the solution, and add 10 ml of standard solution to the mark (1/mL). Accurately pipette 10 ml of standard solution overnight, place in a 10 ml container, dilute with water to the mark, and dilute to the mark: 10 μl of standard solution per liter, 4.1 Common laboratory equipment.
4.2 Spectrophotometer.
5 Steps
5.1 Test group treatment
5.1.1 Collect the average sample of each food, g~.! -- or more than 2 ml of wet sample is placed in a 100 ml incubator, add 3 mL of the sample, and digest with 3 mL of high molecular weight acid. The digestion solution in the flask is initially brown-black. When the solution becomes a colorless or slightly yellow liquid, cool it down completely. Add 2 ml of water to the 100 ml volumetric flask, wash it several times with water, and then transfer it to a volumetric flask. Add water until the bottom is marked and it flows. This solution is the test solution*
GB/T 5009.87—2003
5.2. Take the sulfur model with the digestion formula, and accurately pipette 0.0.3, 1.), 2.0, 7.0, 4.0, 5.0.1, 0, 5, 10, 2030, 40.50g of standard sulfuric acid concentration into a 2ml test tube respectively. Add 2ml of key to dissolve the sulfur in turn, set aside for 4 seconds, add 1ml of sodium dextrose, add x to the scale, and add a spoon. 0.5h after the first test, measure the absorbance at 60nm wavelength with a spectrophotometer, and use the absorbance of 1 μl to observe the phosphorus content and draw a standard curve: 5.3 Accurately determine the test group? 1 μl and the blank liquid (1 μl) are placed in 2 μl test tubes respectively. Only the same operation steps as 15.2 are required to infer the curve. The measured phosphorus content must be obtained by the standard formula (5.4). Where:
Phosphorus price per gram 00
221:
11 The standard is obtained by the same method or by calculating the quality of the sample, the unit is mxV The total volume of the sample is in liters [! .]V:- Determination of the volume of digestive fluid, the unit is liter (m.1): the mass of the sample, the median is grams)
The calculated result is guaranteed to be a valid number.
6 Precision
The absolute difference between two results obtained under the condition of 1 year should not exceed 5% of the arithmetic mean. The second method is molecular absorption spectroscopy
7 Principle
After the organic aldehydes in food are destroyed, they combine with phosphates under acidic conditions to form a blue compound, which is then reduced to phosphates when decomposed into phosphates. Monitor the color and the content of sulfide, and then perform colorimetric analysis: reagent B: 8, 1 acid: 1, 2 sulfur: 1, 81, 1, 15 ml of 15% sulfur solution of 1% sulfuric acid, add to 1 ml of water and mix. After cooling, dilute with water: take 5 ml of 1.5% sulfur solution, add to 91% water and mix. After cooling, dilute with water: take 2 ml of 1.63% sulfur solution, add to 1 ml of water and mix. After cooling, dilute with water: take 1 ml of 1.5% sulfur solution, add to 91% water and mix. After cooling, dilute with water: take 2 ml of 1.63% sulfur solution, add to 1 ml of water and mix.
BB chloride silver neck acid skin take 1 bottle of SC.2H.U. sulfuric acid book HNHH.) add S hoof bomb liquid and press head to 100mI. Put the liquid in a brown bottle and keep it in the refrigerator for at least one month..9 Please prepare the standard, accurately weigh the degradable element 1:01 ml. In a container, add water to the scale, each containing 100 mg of aldehyde, place the bottle in ice for the first time.1 Phosphorus standard solution: bring pound absorption concentrated phosphorus standard reserve solution, CC TnL-1℃2 m1. Apply 1:, use water to change the solution to 10 liters,
9 collector
produce light virtual meter.
10 Analysis steps
10.1 Sample treatment
BT5009.872003
Weigh all kinds of drugs and mix them evenly (about 10).5g wet weight, add 15L nitric acid, 2L high acid, and 2L standard spoon. Heat the liquid in the digestion bottle on a hot plate or electric stove over low heat until it reaches the standard color. Add more acid to the bottle until it is completely dissolved. Increase the heat until the digestion produces a thin, dense oil, which is clear or slightly chromatic. Let the digestion liquid cool, add 20ml of this. After cooling, transfer to 10C.ml. volume, add more water to wash the solution, add the washing solution to the volume of the volume bottle, and draw to the mark: standard: as the sample solution.
Or use the same method to make a blank solution of the reagent: 10.2 standard labor report
Take the phosphorus cup and use the standard of 0.0.2.0.4.0.63.8.1.0ml1. Equivalent to 10 g). Add 1.ml of water to each 25ml colorimetric tube, 2.5ml of chromium-containing solution 2M sodium hydride solution and 5ml of C.5 water to 25mL, place in room temperature for 20min: later. Use a 2cm colorimetric car at 660am length, with a zero tube as a reference, and measure the absorbance at the specified head at 1.0, and use the absorbance barrier to make a standard line. 10.3 Add 1 ml to 2 ml of the test sample and an equal amount of reagent into 25 ml of colorimetric medium, approximately 15 ml of water, 2 ml of 1.5% carrier solution, 2 ml of amino propoxide solution and 0.5 ml of heparin sulfate mixture, and add all together to make up to 25 ml. After standing at room temperature for 2 cm, use 2 colorimetric cups, use 0.1 cm as reference, and measure the common light standard on the spectrophotometer. The measured absorbance is calculated by the standard blue line: 1:11 formula (2), where: X--the content of the sample, unit: 100 g (a00); the amount of carbon in the test solution obtained by the system, unit: μg); the mass of carbon in the blank solution, unit: 100 g (a00); the mass of the sample, unit: 100 g (a00); the volume of the test solution, unit: 100 g (a00); the volume of the blank solution, unit: 100 g (a00); the mass of the sample, unit: 100 g (a00); the volume of the test solution, unit: 100 g (a00); the volume of the blank solution, unit: 100 g (a00); the volume of the test solution, unit: 100 g (a00); the result is calculated to two significant figures.
12 Density
The absolute difference between two independent determination results obtained under the repeatability conditions shall not be calculated as the average value. Method III Determination of phosphate in food
13 Principle
The phosphate in the sample is reacted with ammonium phosphate as an acid to form a yellow phosphate, which can be converted into a blue color by oxidizing. It is called phase blue. The lightness of the blue color is proportional to the phosphate content. 14 Reagents
14.1 sieve hydrochloric acid (1-600 μl).
4.2 Acid solution (5V/): 25% ammonium hydroxide is dissolved in 300ml water. Dissolve 75L concentrated sulfuric acid in water and dilute to 1L with water. Add 50mL 14.3 Hydrogen (terephthalate) ion (5/): Weigh 9.5g of hydrogen (terephthalate) and dissolve in 10ml water. Add 50mL of water. 14.3 Standard ion solution (200E/1): Take 28% sodium thiourea and dissolve in 1UU hot water. Add 2 drops of sodium thiourea before testing. Otherwise, the solution may become slightly mixed. 14.5 Standard ion solution: Take 67165% polyoxyethylene dihydrogen ion (KH2PO4) in a 100cm volumetric flask and add water to make it thick. The wavelength of this wave is equal to 533 nm, and 1.0 ml of this solution is taken. Place it in a 50 μm container and add water to the solution. This solution is equivalent to 1 g of basic acid (PO4-). 15 analysis steps
15.1 Standard curve drawing
Take 1 ml of phosphate solution (equivalent to 10 ml of dry basic acid) 0.0.2.9.4.0.5.0.8.3 ml, divide it into 1 and 2 ml 1. In this colorimetric tube, add 1 ml of iridium phase solution, 200/1. sodium sulfite solution, 1 ml of diphenol solution, filter and dilute to the mark with filtered water, add and adjust for 30 min. Use zero-rate solution as blank and compare the color at 65°C on the spectrophotometer. Determine the optical density of the standard solution and prepare the standard line. 15.2 Determination of the difference between the two standards 15.2.1 Place the ceramic transmitter in a Heat with fire, cool, weigh a spoonful of test sample, and burn it on fire to form charcoal. Then reduce the temperature at 550°C until the ash content is small (if necessary, add concentrated nitric acid to moisten it, which can promote the oxidization of the sample). Add 10 ml of olefin (11). Add all drops of ether (11). Drain it in water and add 3 ml of ether (11). Wash it with water several times. After washing, put it into a 100 ml container. Without release to the degree, refer to filtration (if there is no anti-filtration, no filtration is required), 15.2.2 0.1% of the solution is added to 25% of the colorimetric solution (depending on the phosphorus content), add 2ml of phthalic acid solution, and then add 1% of the sodium ion solution. When the sodium ion solution is 290g/mL, the hair will start to work. Based on the light measured, the light from the standard line is calculated. The result is calculated as
, see formula (3) -
x- n ×1 3
Wu Zhong:
X-\ The sample contains 4 grams of acid salt (PO4) per gram of protein (kg). The unit is the amount of the sample absorbed during the determination, in grams (). The result is calculated to be a two-digit valid number. The difference between the two independent determinations obtained in the repeated determinations shall not exceed the technical level. 6,dAdd all the succinic acid to the water solution and add 3ml of 11% succinic acid. Wash with water several times. After the peak is washed, the residue will be filtered (if there is no anti-filter, no filtration is required). 15.2.2 Add 0.1% succinic acid solution to 25% dichromatic agarose (depending on the phosphorus content) and add 2ml succinic acid solution. Then, add 1% succinic acid solution to the water ... 3
Wu Zhong:
X-\The sample contains 4 grams of protein per kg of the standard salt (PO4). The unit is the amount of protein absorbed by the sample during the determination, in grams (). The result is calculated to two significant figures. The difference between the two independent determinations obtained in the repeated determinations shall not exceed the technical average. 6,dAdd all the succinic acid to the water solution and add 3ml of 11% succinic acid. Wash with water several times. After the peak is washed, the residue will be filtered (if there is no anti-filter, no filtration is required). 15.2.2 Add 0.1% succinic acid solution to 25% dichromatic agarose (depending on the phosphorus content) and add 2ml succinic acid solution. Then, add 1% succinic acid solution to the water ... 3
Wu Zhong:
X-\The sample contains 4 grams of protein per kg of the standard salt (PO4). The unit is the amount of protein absorbed by the sample during the determination, in grams (). The result is calculated to two significant figures. The difference between the two independent determinations obtained in the repeated determinations shall not exceed the technical average. 6,d
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