NY/T 1601-2008 Determination of Phoxim Residues in Fruits by Gas Chromatography NY/T1601-2008 Standard download decompression password: www.bzxz.net
This standard specifies the gas chromatography method for the determination of phoxim residues in fruits. This standard is applicable to the determination of phoxim residues in fruits.

CS 67.080.10
Chinese Standard
NY/T1601—2008
Determination of phoxim residues in fruits
Gas chromatography
Determnination of phoxim residues in fruitsGas chromatographry
Published on 2008-05-16
Implemented on 2008-07-01
Published by the Ministry of Agriculture of the People's Republic of China
This standard is issued by the Ministry of Agriculture of the People's Republic of China and is under the jurisdiction of the Department of Agriculture of the People's Republic of China 160)--2008
This standard was drafted by: Fruit and Vegetable Quality Supervision and Inspection Center (Xingcheng), Ministry of Agriculture, Institute of Chinese Agricultural Sciences. The main drafters of this standard are: Nie Jiyun, Li Jing, Shen Banyin, Xu Guofeng, Hai Fei, Shuo Yonglong, Zhen Xu, 1 Scope
Determination of Phoxim Residues in Fruits
Gas Chromatography
This standard specifies the gas chromatography method for the determination of phoxim residues in fruits. This standard is applicable to the determination of phoxim residues in fruits. The detection limit of this standard method is c.02mg/kg. 2 Normative References
NY/T 1601-2008
The clauses in the following documents become the clauses of this standard through the reference of this standard. For all referenced documents of the current period, all amendments (excluding errors) or revised versions thereof are not applicable to this standard. However, the parties concerned may study whether the latest versions of these documents can be used in accordance with the agreement reached between the parties. For all undated referenced documents, the latest version shall apply to this standard. NY/T789 Sampling method for pesticide residue analysis samples 3 Principle
The chlorinated phosphorus in the sample is extracted with acetonitrile, and the extract is purified and concentrated, and then detected by gas chromatography (flame photometric detector, phosphorus filter: 526 nm). The external standard method is:
4 Reagents and materials
Unless otherwise specified, all water used is distilled water, and all reagents used are analytically pure reagents. 4.1 Preparation.
4.2 Internal reaction: redistilled when necessary, no interference was detected, 4.3 Sodium oxide: baked at 10℃ for 4h
4.4 Phoxim standard: concentration 256%.
4.5 Preparation of thiophosphorus standard solution: Prepare 100 mg/l standard solution with chloramine and store it in a bottle below -18°C. When used, dilute it with an internal viscometer to make a 0.m standard working solution. 5 Instruments and equipment www.bzxz.net
5.1 Gas chromatograph: equipped with flame photometric detector (FPD).
5.2 Tissue crusher.
5.3 Homogenizer.
5.4 Vortex mixer
5.5 Alpha blowing machine.
5.6 Centrifuge: 4 500 -/min.
EAnalysis steps
6.1 Sample preparation
According to NY/T789, take a sample and gently wipe off the attachments of the sample container with dry gauze. Take the edible part, quarter it, cut it into pieces, and use a NY/T16012C08 machine to remove the grape pulp.
6.2 Extraction
Weigh the fruit and weigh 20.0 (accurate to 0.01) in a 100ml centrifuge tube, add 20.0mL of acetonitrile: homogenize with a sonicator for 2min, add 3g~g sodium sulfite, homogenize for 1min, centrifuge at 3000r/min for 5min, and clarify. 6.3 Concentrate| |tt||10.0ml of liquid (6.23 microliters above 10m. scale), blow to nearly dry with 40℃ air, adjust to 2.0mL, 6.4 Determination
6.4.1 Chromatographic reference conditions
6.4.1.1 Chromatographic column
100% poly (R1x-1) silica capillary non-ferrous metal, 15.0m, 0.53mm×1.5μm, or. 6.4.1.2 Temperature
Inlet temperature: 190℃;
Drag temperature: 250℃
Excitation sequence: 50℃ (hold for] min) 30℃/150℃ (hold for 10 min) mia)/mz-190℃ (maintain for 5min). 6.4.1.3 Gas and flow
Gas: argon, pure 99.999%, flow rate 25mL/min. Fuel gas: hydrogen, pure 99.999%, flow rate 100nL/min. Auxiliary combustion gas: air, flow rate [mL/min. 6.4.1.2 Sampling method
Non-split flow injection.
6.4.2 Qualitative determination
The retention time of the non-toxic components of the sample is determined by the retention time of the sulfur standard substance within ±0.05mn.
6.4.3 Qualitative determination
Take 1. Test solution and the corresponding standard working solution, integrate the chromatographic peak area, quantify by external standard method, and the standard working solution The value of phoxim in the sample solution should be within the linear range of the instrument detection. Simultaneously, a close experiment is performed. 7 Calculation of results
The phoxim residue in the sample is calculated according to formula (1). =PXAXVIXV:
W||W--- the residual phoxim, unit is gram per dry gram (mg/kg); α\ mass concentration of the phoxim standard solution, unit is gram per liter (m/L); 4 The peak product of phoxim in the sample, integration unit; V--- the total volume of the reagent, unit is whole liter (nl); V--- the volume of the sample solution, unit is filter liter (mL): A: sample mass, unit is gram ()
A--- the peak product of the standard working solution of phoxim, integration unit: V--- the volume of the test, unit is milliliter (ml) The calculation result is the three-digit effective value.
8 Precision
NY/T160—2008
The standard solution of chlorpyrifos pesticide was added to fruits at three levels of 0.c21ng/kg, 0.05mg/kg and 0.1mg/kg to carry out the precision test of the method. The addition recovery density of the method is 80%120%. The absolute difference of independent test results obtained under the renaturation conditions shall not exceed 5% of the arithmetic mean. Chromatogram
1 Agent:
Xinzhu Research and Development Time 15 r.36.
Chart Chromatographic separation diagram
NY/T1601-2008
People's Republic of China
Agricultural industry standard
Determination of mercaptophos residues in fruits
Gas chromatography
NY/T 160I-—2008
Published by China Agriculture Press
(Building 18, Biaoliaodian Street, Dianyang District, Beijing) (Postal Code: 100125
Website: tcagl.com.cn)
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Xinhua Bookstore: Beijing Distribution Office Distributed by Xinhua Bookstores in various places Format 880mum×1230m1/36
First edition in June 2008
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June 2008, Beijing, first printing
Book number: 16109:1664
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