This standard specifies the HPLC method for the determination of fomesulfuron residues in soybeans and cereals. This standard is applicable to the determination of fomesulfuron residues in soybeans and cereals. The detection limit of this method is 0.02 mg/kg; the linear range is 5 ng to 320 ng. GB/T 5009.130-2003 Determination of fomesulfuron residues in soybeans and cereals GB/T5009.130-2003 Standard download decompression password: www.bzxz.net

ILS67,040
National Standard of the People's Republic of China
GB/T5009.130--2003
Substituted for GBT16337105
Determination of fomesafen residues in soyheans and cereals cereals2003-08-11 Issued
Ministry of Health of the People's Republic of China
National Standardization Administration of China
2004-01-01 Implementation
GB/T5009.130—2003
This standard replaces GB/T16337·1996* Determination of flusulfuron residues in total soybean grains 3. This standard is in accordance with GB/T20001.4-2501 Standardization Rules Part 4, Chemical Analysis Methods. The structure of the original standard has been modified.
This standard was proposed by the Ministry of Health of the People's Republic of China and was drafted by: Beijing Municipal Health and Epidemic Prevention Station, Food Hygiene Supervision Institute of the Ministry of Health, Beijing Institute of Food Industry. The main contributors of this standard are Dan Mijiang, Wu Guobi, Zhang Rong, Fang Congchuan, and Tu Tianli. The original standard was first issued in 1556. This standard is the first sample order. 142
GH/T 5009,13D—2003
Determination of chlorsulfuron residues in soybeans and cereals This standard specifies the HPLC determination method for chlorsulfuron residues in soybeans and cereals. This standard is applicable to the determination of chlorsulfuron or chlorsulfuron in soybeans and cereals. The detection resistance of this method is 0.02g/kg! The linear range is 5g-320:2 Principle
Ammonia sulfamethoxam in the sample is organically collected under acidic conditions, and after liquid-liquid distribution and carbonyl adsorption column purification to remove interfering substances, it is determined by high performance liquid chromatography-ultraviolet detection. The qualitative analysis is based on the retention time of the chromatographic peak, and the quantitative analysis is based on the external standard method. 3 Wuzhou
3.1 Methylthiocyanate (chromatographically pure>.
3.2 Ethyl acetate: redistilled.
3. 3. Chloroform,
3.4 ​​Pre-treat the carbon absorbent with ≤ml trichloromethane before use. 3.5 Hydrochloric acid (83nL/L): Take 8.3ml of hydrochloric acid and dilute to 10CmL with water. 3.6 Sodium hydride solution (1.0g/L): Take 0.4g of sodium hydride and add it to water, dilute to 1UmL. 3.7 Sodium hydroxide solution (20g/L): Take 20) sodium sulfate + and dissolve it in water, dilute to 1000mT, use sodium hydroxide solution (3.S) to adjust pH = 11.
3.8 Propane solution, take 98mT of propane and mix with (re-distilled catalase). 20mL hydrochloric acid. 3.9 Methanol-trichloroethane (3+7)
3.10 HPLC mobile phase (methanol 0.01mol/L sodium acetate = 60+40. pH 3.2). Weigh 0.544g of product ethyl acetate (CHCOUN·3HO) and dilute to 400L with water. Add 24ml methanol (3.1) and mix well. Adjust pH to 3.2 with phosphoric acid (super pure). Filter through U.Em microfilter and degas with ultrasonic. Flow rate 1.6 rmL/min3.11 Fluorosulfuron standard stock solution: Weigh 0.100 μL of fluoxetine (omcsafen, purity 98%). Place in a 100 μL container: Dissolve in methanol 3.1) and add 1.00ul of the solution to be tested. Contains 1.8g of chlorosulfonaldehyde. 3.12 Standard use of sulfanilamide: Pipette 5.0L of sulfanilamide standard stock solution (3.11) in 5C.Cml, add methanol (3.1) to the solution to make it up to 1.0ml. Contains 1009.0% sulfanilamide. Stable for 4 weeks. 4.1 High-efficiency phase spectrometer (with UV detector) 4.2 Analyzer. 4.3 Electric heating water. 4.4 Other required triangular flask: 250mL. 4.5 Sensor: Hyaluronic acid core funnel (C; 1C mL) extraction bottle (100lrml.). 4.6 Separation funnel 250ml.
4.7 Syringe: 10ml.,
GB/T5009.130-2003
5 Analysis stepsbzxZ.net
5.1 Sample preparation
5.1.1 Extraction: Pass the test powder through a 20% sieve and mix. Weigh about 20g of the sample accurately to C.0C1 and place it in a flask, add 100mL of acetaldehyde, shake on a shaker for 15min, separate the layers, take the upper layer and filter it. 5.1.2 Purification: Take 100mL of the filtrate and put it into a funnel, add 100mL of sodium hyaluronate, adjust the H2O to 10·~ with sodium hydride solution, add 50mL of acetaldehyde, separate the layers: discard the upper acetaldehyde. The following is to adjust the H2O volume to 1-2, with 507% energy, until stratification, the lower layer is dropped and then added with ZrO2, and the mixture is combined and allowed to stand for 15min. The water layer is collected and placed in electric constant temperature water until nearly 3min. The decomposed liquids in trichloroethane are combined and transferred into an injector connected to the purifier, and the sample is slowly passed through the injector. The purifier is rinsed with 10mL of trichloroethane and the elution wave is removed. Eluted with 2mL of undecylamine, the eluted liquid is collected in a stream, evaporated in electric constant temperature water until nearly dry, poured into a graduated centrifuge tube with a small amount of methyl ether, and adjusted to 1.0L of liquid for chromatographic separation.
5.2 Determination
5.2.1 Chromatographic reference method: UV detector wavelength 299nm, 0.01ArS. Xenotron, octadecyl silica gel phase 200m long. Inner diameter 4.5nm
5.2.2 Standard solution: Take 0.50, 1.02.0, .0, 8.0CrmI iodine sulfoxide standard solution in 5 100.0T1 blood bottles, add chloramine to dilute to the scale, the concentration of fluazifop in this standard series is 0.5.1.0, 2.0.2.0.8.0g/ml respectively, and this calibration is freshly prepared. Collect 10 micrograms of sample at each micrometer, and use the concentration of 1% hydroxylamine monoaldehyde as the calibration curve. The peak height is the Kjeldahl coordinate system.
5.2.3 Standard curve: Calibrate the hydroxylamine monoaldehyde. This curve is shown in Figure 1a. 54
5.01. 02. 03. 0 4.0 5. 0 8.0 7.08. 0 5.2.4 Chromatography: Take 1% hydroxylamine monoaldehyde and inject it into the phase chromatograph. Record the chromatographic time and sieve height. Use the chromatogram to determine the concentration of hydroxylamine monoaldehyde. According to the chromatogram, the amount of hydroxylamine monoaldehyde can be found out from the standard curve. 5.2.5 Single spectrum: The standard chromatogram of hydroxylamine monoaldehyde is shown in Figure 2. un
Leave 2 according to the standard chromatographic run of sulfonamide
Conclusion calculation
The content of chlorsulfamide in the test sample is calculated as follows: xv
Play a,
(. The content of chlorsulfamide in the test sample, the unit is gram you call complete (mgkg): ---The concentration of sulfonamide in the sample extraction chain, the unit is microgram milliliter (g/ml.):.-The purified volume is milliliter (T.) V.-..-The volume of the microfiltration stabilized is milliliter (mL.\The volume of the extracted solution is milliforce (mL>;--The amount of sample, the unit is gram g>
The calculation result is retained to two significant figures,
The accuracy
GB/T 5009.1302003
The confidence of the two independent results obtained under the condition of multiplex measurement shall not exceed 10% of the arithmetic mean. 267
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