GB/T 5009.221-2008Determination of the residues of diquat in cereals (English PDF)
粮谷中敌草快残留量的测定
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
December 3, 2008
Implementation date
March 1, 2009
Scope
GB/T 5009.221-2008 is the English-translated version of 粮谷中敌草快残留量的测定.
GB/T 5009.221-2008 sets out a method for determining diquat residues in cereals.
Clause 1 states that the standard specifies the method for the determination of diquat residues in cereals and that it applies to the determination of such residues in corn and barley, with a detection limit of 0.005 mg/kg and a linear range of 0.001 mg/L to 0.100 mg/L. The clause printed as Principle 2 describes rapid extraction with 95% ethanol, reaction with sodium borohydride, extraction with chloroform, transfer of the solvent to n-hexane and measurement by gas chromatography with a mass spectrometric detector, selected ion detection being used for confirmation and an external standard for quantification.
Clause 3, Reagents and materials, lists n-hexane, chloroform, sodium borohydride, hydrochloric acid solution, sodium hydroxide solution, anhydrous sodium sulfate, 95% ethanol solution and a diquat dibromo salt standard of purity not less than 99%, and gives the preparation and storage of the standard stock solution.
Clause 4, Instrument, calls for a gas chromatograph-mass spectrometer with an EI source, a rotary evaporator, a vortex mixer, flat-bottomed flasks of 100 mL and 50 mL, a 125 mL funnel and a high-speed disperser homogenizer.
The clause printed as Step 5 Analysis opens with 5.1 on extraction and purification, working on a 5 g milled sample passed through a 2.0 mm round-hole sieve, but the draft version on the page breaks off in mid-sentence inside that subclause, so the calculation and the rest of the method are not shown.
The foreword declares Appendix A an informative annex and states that the standard was proposed and administered by the Ministry of Health of the People's Republic of China.
The page gives ICS 67.040 and Chinese classification C53. It was issued on 2008-12-03 and has applied since 2009-03-01.
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Document preview — GB/T 5009.221-2008
National Standard of the People's Republic of China
- ICS
- 67.040
- Classification
- C 53
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Principle
- 3 Reagents and materials
- 4 Instrument
Foreword
Appendix A of this standard is an informative annex.
This standard is proposed and administered by the People's Republic of China Ministry of Health.
This standard by the People's Republic of China Ministry of Health is responsible for interpretation.
1 Scope
This standard specifies the method for determination of Cereals by diquat residues.
This standard applies to corn, barley diquat determination of residues.
The standard detection limit of 0.005mg/kg, the linear range of 0.001mg/L ~ 0.100mg/L.
2 Principle
According diquat solubility and stability, diuron extracted with 95% ethanol fast, and after the reaction of sodium borohydride, extracted with chloroform, except To chloroform to normal hexane, gas chromatography - mass spectrometry detector measurement, external standard, using selected ion detection for confirmation and Quantified.
3 Reagents and materials
Unless otherwise specified, all reagents shall be of analytical grade (organic solvent to be re-distilled) water as a water (conductivity 25 °C <=0.01mS/m).
3.1 N-hexane (C6H14).
3.2 Chloroform (CHCl3).
3.3 Sodium borohydride (NaBH4).
3.4 Hydrochloric acid solution. 2mol/L.
3.5 Sodium hydroxide solution. 5mol/L.
3.6 Anhydrous sodium sulfate (Na2SO4). After 650 °C burning 4h placed in the dryer.
3.7 95% ethanol solution.
3.8 diquat salt dibromo standard. Purity >=99%, CAS 6385-62-2 is.
3.9 diquat standard solution. Accurately weigh an adequate amount of diquat dibromo salt standard, accurate to 0.0001g, dissolved in water after 1mL 95% ethanol solution formulated at a concentration of 100µg/mL standard stock solution, if necessary adding a suitable concentration of the working standard solution, Paul 4 °C stored in the refrigerator, use 90d.
4 Instrument
4.1 Gas chromatography - mass spectrometry. Hotels (EI source).
4.2 Rotary evaporator.
4.3 Vortex mixer.
4.4 Flat-bottomed flask. 100mL.
4.5 Flat-bottomed flask. 50mL.
4.6 Funnel. 125mL.
4.7 High-speed disperser homogenizer.
5 Analysis
5.1 Extraction Purification
Weigh milled mix (over 2.0mm round hole sieve) Sample 5g (accurate to 0.01g) in 100mL flat-bottomed flask, 30mL 95% ethanol solution, homogenized 3min. Hydrochloric acid was added 4mL 50mg of sodium borohydride was added, the oscillation 40min (2mol/L) was treated with 5mL95% ethanol solution, rinse the flask and suction filtered twice. The filtrates were combined in a water bath at 35 °C ethanol was removed by rotary evaporation, the residual aqueous layer was transferred to […]
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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