GB/T 21925-2008Determination of herbicide residues in water - LC/MS method (English PDF)
水中除草剂残留测定 液相色谱/质谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
May 16, 2008
Implementation date
November 1, 2008
Scope
GB/T 21925-2008 is the English-translated version of 水中除草剂残留测定 液相色谱/质谱法.
This standard sets a liquid chromatography/mass spectrometry method for determining herbicide residues in water.
Clause 1 states that it covers the residues of the triazine herbicides atrazine, simazine and prometryne and of the phenylurea herbicides chlorotoluron and isoproturon, that it applies to irrigation water, surface water, ground water and other water, and that the detection limit is 0.05 micrograms per litre for prometryne and 0.25 micrograms per litre for atrazine, simazine, chlorotoluron and isoproturon.
Clause 3, Principle, has these herbicides taken from the water by liquid-liquid extraction and concentration or through a solid phase extraction cartridge with purification and elution, and then quantified on line by liquid chromatography/mass spectrometry.
Clause 4, Reagents and materials, calls for analytical grade reagents and twice-distilled ultra-pure water and lists chromatographically pure methanol, acetonitrile and acetone, dichloromethane, formic acid, an aqueous solvent microfiltration membrane of 0.45 micrometre pore size, standard samples of the five herbicides at 100 micrograms per millilitre, and a series of mixed standard solutions from 5 to 500 micrograms per litre prepared in acetonitrile and kept in the dark at 4 degrees Celsius.
Clause 5, Apparatus, requires a liquid chromatograph/mass spectrometer whose ion source is atmospheric pressure electrospray ionization, an SB-C18 100 mm by 3.0 mm by 3.5 micrometre column or an equivalent polar column, a solid phase extraction column of the SDB 500 mg/3 mL or SDBC18 1000 mg/6 mL type or equivalent, a rotary evaporator and dry nitrogen; the draft breaks off at the end of this list.
The table of contents gives the rest of the standard as a clause 6 whose heading the draft garbles, then Procedure, Calculation Results and Precision, followed by two informative annexes holding the total ion chromatogram and the spectra of the five herbicide standard substances.
Clause 2 cites GB/T 12998 and GB/T 12999. The standard was drafted by the National Agricultural Processed Food Quality Supervision and Inspection Center and the Anhui national agricultural standardization and monitoring center.
The page shows no earlier edition; it was issued on May 16, 2008 and has applied since November 1, 2008.
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Document preview — GB/T 21925-2008
National Standard of the People's Republic of China
- ICS
- 13.060.50
- Classification
- Z 16
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Preface
- 1 Scope
- 2 Normative references
- 3 Principle
- 4 Reagents and materials
- 5. Apparatus
- 6 is recommended to use the instrument for
- 7 Procedure
- 8 3 Calculation Results
- 9 Precision
- Appendix A (informative) Five Kinds of Herbicide Standards LC/MS total ion chromatogram
- Annex B (informative) Five Kinds of Herbicide standard substance spectrum
Foreword
The Standard Appendix A, Appendix B is an informative annex.
This standard by the State Administration of Quality Supervision Inspection and Quarantine of People's Republic of China, China National Standardization Management Commission. This standard by the Standardization Administration of China.
1 Scope
This standard specifies the water triazine herbicides atrazine, simazine, Prometryne and phenylurea herbicide chlorotoluron, isoproturon herbicides Residues of liquid chromatography/mass spectrometry.
This standard applies to the determination of irrigation water, surface water, ground water and other triazines and phenyl urea herbicide residues.
The detection limit of this standard. Prometryne was 0.05µg/L, atrazine, simazine, chlorotoluron, isoproturon was 0.25µg/L.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 12998 Quality Guidance on sampling techniques Conservation and management of technical requirements
GB/T 12999 Water Sampling sample
3 Principle
Water triazine herbicides atrazine, simazine, Prometryne and phenylurea herbicide chlorotoluron, isoproturon, etc., by liquid-liquid extraction, concentration Or SPE solid phase extraction cartridge, purification, elution, online quantitative analysis by liquid chromatography/mass spectrometry (LC/MS).
4 Reagents and materials
Unless otherwise indicated, the reagents used were of analytical grade, ultra-pure water for the second distillation.
4.1 Methanol. chromatographically pure.
4.2 Acetonitrile. chromatography.
4.3 Acetone. chromatography.
4.4 Dichloromethane.
4.5 Formic acid (85%).
4.6 Solvent microfiltration membrane (aqueous), pore size 0.45µm.
4.7 Standard sample. atrazine, simazine, Prometryne, chlorotoluron, isoproturon (concentration 100µg/mL).
4.8 Standard solution. preparation of standard samples with acetonitrile as the standard stock solution, diluted stock standard solution as a single ingredient concentration 5µg/L ~ 500µg/L mixed standard solution series (mixed standard solution in the dark at 4 °C, you can use a month now with the current recommendation).
5 Apparatus
5.1 Liquid chromatography/mass spectrometry (LC/MSD), the ion source is atmospheric pressure electrospray ionization (API-ESI).
5.2 Columns. SB-C18 100mm x 3.0mm x 3.5µm or equivalent polar column.
5.3 Solid phase extraction column. SDB 500mg/3mL or SDBC18 (1000mg/6mL) or equivalent person.
5.4 Rotary evaporator.
5.5 Meter dry nitrogen.
......
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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