SN/T 3860-2014Determination of pymetrozine residues in food for export - LC-MS/MS method (English PDF)

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules.

This standard is proposed and managed by the National Certification and Accreditation Administration Committee.

This standard was drafted. People's Republic of China Shaanxi Exit Inspection and Quarantine.

1 Scope

This standard provides the food for export pymetrozine residues in liquid chromatography - mass spectrometry/mass spectrometry methods.

This standard applies to apples, peaches, rice, corn, almonds, spinach, milk, eggs, pork, liver in pymetrozine residues and determination Confirmed.

2 Method summary

Sample of pymetrozine with 1.9 ammonia - acetonitrile extracted by solid phase extraction (SPE), liquid chromatography - mass spectrometry/mass spectrometry, External standard.

3 Reagents and materials

Unless otherwise indicated, the reagents used were of analytical grade water for ultra-pure water.

3.1 acetonitrile. HPLC grade.

3.2 Methanol. HPLC grade.

3.3 hexane. HPLC grade.

3.4 sodium chloride.

Ammonia 3.5. mass fraction of 25% to 28%.

Ammonia 3.6. 0.2%, taking 4.0mL aqueous ammonia (3.5), diluted with ultrapure water to 500mL, and mix.

3.7 ammonia - acetonitrile (1090, volume ratio). Take 100mL ammonia (3.5), was added 900mL of acetonitrile (3.1) and mix.

3.8 hexane saturated acetonitrile solution, take 200mL hexane (3.3) in 250mL separatory funnel, was added a small amount of acetonitrile (3.1), severe vibration Shake a few minutes, still hierarchical, discarding the lower acetonitrile layer, that is, too.

3.9 aqueous methanol (1090, volume ratio). Take 100mL methanol (3.2), was added 900mL ultrapure water and mix.

3.10 pymetrozine standards (pymetrozine, C10H11N5O, CAS number. 123312-89-0). purity of greater than or equal to 99.9%.

3.11 Standard stock solution. Weigh accurately a certain amount of pymetrozine standard (3.10), dissolved in methanol, dubbed 1000mg/L standard stock Liquid, following -18 °C stored.

3.12 standard solution. accurate Pipette stock standard solution (3.11) 1.0mL in 100mL brown volumetric flask with methanol to carve the degree of concentration of 10.0mg/L, stored in the dark at less -18 °C.

3.13 matrix standard solution. Pipette different volumes of standard working solution (3.12), with a blank sample extract dubbed the concentration of 5ng/mL, 10ng/mL, the matrix standard solution 25ng/mL in. Using now.

3.14 C18 solid phase extraction column. 500mg, 3mL.

4 Instruments and equipment

4.1 Liquid chromatography - mass spectrometry/mass spectrometry. Distribution ionization (ESI).

4.2 Electronic balance. a sense of the amount of 0.1mg and 0.01g.