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1 Scope
This part of SN/T 1737 specifies the residues of pyrazolone, chlorfenapyr, cycloxydim, clethodim, sethoxydim, fenbuprofen, triclotrione and cyclooxydione in imported and exported foods Methods for determination and confirmation of liquid chromatography-mass spectrometry/mass spectrometr.
Pyramidone, Cycloxazone, Clethodim, Sethoxydim
This section applies to rice, soybeans, pork, beef liver, chicken liver, milk, orange, blue poison, spinach, onion, walnut kernel, pyrazolone, chlorfenapyr, eagletrione, clethodim, dilute in tea Determination of the residues of chlorfenapyr, fenbuprofen, triclotrione and cyclofenazon.
triclotrione cyclobenzotrione
2 Method summary
The residual cyclohexenone herbicides in the sample were extracted with acidic acetonitrile or acetonitrile, and the extract was purified by N-propylethylenediamine (PSA), octadecylsilane (ODS) and graphitized carbon black, and the liquid Phase chromatography-mass spectrometry/mass spectrometer detection and confirmation, external standard method for quantificatio.
Octadecylsilane
3 Reagents and Materials
Unless otherwise specified, all reagents are of analytical grade, and the water is first-grade water specified in GB/T 6682.
1 Acetonitrile: chromatographically pur.
2 Acetic acid (95%.
3 Formic acid (80%.
4 Sodium acetat.
Sodium acetate
5 Sodium chlorid.
6 Anhydrous magnesium sulfate: calcined at 650℃ for 4h, and placed in a desiccator for later us.
Anhydrous magnesium sulfate
7 1% acetic acid acetonitrile solution: take 10 mL of acetic acid (2), add 990 mL of acetonitrile (1), and mix wel.
8 60% acetonitrile aqueous solution: take 60 mL of acetonitrile, add 40 mL of water, and mix wel.
9 Formic acid-aqueous solution (2+998, volume ratio: take 2 mL of formic acid (3), dissolve in water and dilute to 1 000 m.
10 Cyclohexenone standard: clethodim (Clethodim), CAS number: 99129-21-2, purity greater than or equal to 99%; Tepraloxydim, CAS number: 149979-41-9, purity greater than or equal to 99% Equal to 99%; Cycloxydim (Cycloxydim), CAS number: 101205-02-1, purity greater than or equal to 95%; Trakoxydim (Tralkoxydim), CAS number: 87820-88-0, purity greater than or equal to 95%; Alloxydim-sodium, CAS number: 55635-13-7, purity greater than or equal to 98%; Pro-foxydim-lithium, CAS number: 139001-49-3, purity greater than or equal to 95%; Butroxydim, CAS number: 138164-12-2; purity greater than or equal to 99%; Sethoxydim, CAS number: 74051-80-2, purity greater than or equal to 99.
pyrazolone
11 Standard solution:
11 Standard stock solution of cyclohexenone: Accurately weigh an appropriate amount of standard cyclohexenone, dissolve it with acetonitrile and dilute to a 100 mL brown volumetric flask to obtain a standard stock solution with a concentration of 100 ug/mL , store this solution away from ligh.
12 Mixed standard intermediate solution: Accurately pipette 5 mL of each standard stock solution of cyclohexenone into a 50 mL brown volumetric flask, and dilute with acetonitrile to form a mixed standard intermediate solution with a concentration of 0 ug/m.
13 Mixed standard working solution: Prepare an appropriate mixed standard working solution with blank sample matrix before use as require.
12 Graphitized carbon black adsorbent: 120 um~400 u.
13 N-propyl ethylenediamine (PSA) adsorbent: 40 um~100 u.
14 Octadecylsilane (ODS) bonded phase: 40 um~100 u.
15 Aqueous filter membrane: 22 u.
4 Instruments and equipment
1 Liquid chromatography-mass spectrometry-mass spectrometer: equipped with HSI ionization sourc.
2 Electronic balance: Sensitivity 01 mg, 01 .
3 Crushe.
4 Tissue mashe.
5 Centrifuge: 4 000 r/mi.
6 Vortex mixe.
7 Nitrogen blowe.
8 Homogenizer: 10000r/mi.
9 Screw-cap polypropylene centrifuge tubes: 50 mL, 15 m.
10 Glass stoppered centrifuge tube: 15 m.
Related Links: Determination of Diphenyl Ether Herbicide Residues in Grains and Oilseeds by Gas Chromatography/Mass Spectrometry (2)
Determination of diphenyl ether herbicide residues in grains and oilseeds by gas chromatography/mass spectrometry (2)