GB/T 5009.173-2003 Determination of cypermethrin residues in pome and citrus fruits

This standard specifies the determination method of hexythiazolin in pome and citrus fruits. This standard is applicable to the determination of hexythiazolin in pome and citrus fruits. The minimum detection amount of this standard is 0.126ng. The optimal linear range of this method is 1ng～40ng. GB/T 5009.173-2003 Determination of hexythiazolin residues in pome and citrus fruits GB/T5009.173-2003 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
GB/T5009.173--2003
Determination of hexyihiazox residues in pome and eitrous fruits2003-08-11Published
Ministry of Health of the People's Republic of China
National Standardization Administration of China
2004-01-01Implementation
This standard was proposed by the Ministry of Health of the People's Republic of China. GB/T5009.173—2003
This standard was drafted by: the Ministry of Health of the People's Republic of China, the Institute of Science and Technology Information of Jilin Province, and the People's Medical University of Jilin Province.
Drafters of this standard: Ben Yu, Tong Duo, Zhou Li, Liu Hongtao and Chang Xin. GB/T 5009.173—2003
5-(4-Diaminophenyl)-3-(N-dihydrodiphenylamine)-4-methyloxazolidine-2-yl) is a highly effective and low-toxic pesticide widely used to prevent and control pests in apples and citrus fruits. The drug has been approved for use on fruits in my country, and the country has formulated maximum residue standards, stipulating 0.5ng/kg for pears and 0.1ng/kg for oranges. The standard is a supporting method for this. 2
1 Standard
GB/T 5009.173—2003
Determination of chlorpyrifos in pome and citrus fruits This standard specifies the determination method of chlorpyrifos in pome and citrus fruits. This standard is applicable to the determination of chlorpyrifos in pome and citrus fruits. Minimum amount of this standard: 0.126g
Linear range of this standard: 1~40ng2 Principle
The chlorpyrifos prepared in the test sample is extracted and purified, and then determined by high performance liquid chromatography with ultraviolet detector, and compared with the standard solution for qualitative determination.
3 Reagents
3.1 Petroleum ether (process 33℃~60℃).
3.3 Elution agent: petroleum ethyl acetate (99-1). 3.4 Sodium sulfate hydrate was burned at 60 °C for 5 min. 3.5 Phase chromatograph: 7% sodium hydroxide (7030). 3.610/sodium sulfate was added to the solution, 3.7 Sample treatment: PT group adsorption agent: use left olealdehyde-acetic acid (99-1> to elute the pre-treated sample. 3.8 Standard chromatograph: 0.100% hexythiazolidine (hexythiazolidine), calcium concentration>99%, accuracy 0.1%, methanol solution was determined by standard chromatograph, 1 mg/m3 of standard chromatograph. 4 Instruments 4.1 Microchromatograph: H Detector: 4.2 Ultra-clear solution. 4.3 Slurry. 4.4 Thermal analyzer. 4.5 Filter, 5 Analytical steps
5.1 Sample preparation
Take 1.5 g of the homogenized sample and put it in 5 mL of flask, add 2 μL of methanol, mix well and take 20 μL of the extract on a sonicator. Pass the extract through a 125 μm separatory funnel and use 10 μL of methanol to separate the residues. Combine the methanol extracts in a separatory funnel. Add 50 mL of 4 μg/L sodium sulfate solution and 20, 10, and 1 μL of petroleum aldehyde to the separatory funnel. Combine the extracts and add them to a sodium sulfate-free flask. Concentrate to dryness on a flask. 5.2 PurificationWww.bzxZ.net
Transfer the 5 μg concentrate to a treated flask and elute with 20 mL of ethanol (3-1) and collect the eluted extract. Gradually concentrate to nearly +, the effective gas is carefully added, 2ml. alcohol rate solution, passed through 0.4m coal, prepared, 427
GE/T5009.173-2003
5.3 High performance liquid chromatography static test strip
stainless steel column, 200mm×4.6mT, internal adjustment OD9c<); mobile phase, 2 tons of water (7+3u) elution 1ml.mim grid measurement wavelength 225nmr temperature: 2°C. 5.2 Determination
Take 10T. rate end rain standard ticket C, 0.10.0.5C..00.2.00.3,00, 2.00g/mL and sample solution into the liquid chromatograph, record the change in sleep height.
6 Calculate the results
according to the formula Calculation:
Wherein:
functional auxiliary content, unit is milligram per dry gram (mg/kg): G.
the concentration of thiophene calculated from the standard curve, unit is per milliliter (ug/m,) the volume of the purification liquid, unit is milliliter (ml.), the mass of the sample, unit is gram (g),
calculate the effective effect of the two air-conditioning,
7precision
under the condition of multiple control system, the absolute difference of two independent test results shall not exceed 10% of the arithmetic mean 3liquid chromatography reference range
high density phase special parts, stainless steel, 2camm×4.%nml, internal ODsCu: 5u, washing, requires 753 flow rate! l Inspection length 82% m no: 33, Figure 1 Standard spectrum of chloranil || tt || Figure 2 Apple sample free spectrum || tt || Field 3 Apple sample blank spectrum
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