SN 0603-1996Determination of tralomethrin residues in food of plant origin for export. LC-MS/MS (English PDF)

Foreword

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

This standard replaces SN 0603-1996 "Mi Road cereals for export morpholino residues in." this standard compared with SN 0603-1996, in addition to editorial changes, the major technical changes are as follows.

--- Modify the standard name;

--- Expanding the scope of application;

--- Canceled in the sampling method SN 0603-1996;

--- Improved sample pretreatment technology lines.

--- Canceled SN 0603-1996 in GC and GC-MS detection method was confirmed using LC-MS/MS method tralomethrin (Road microphone morpholine, tralomethrin) Residues accurate qualitative and quantitative.

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

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

1 Scope

This standard specifies the botanical foods tralomethrin residues by liquid chromatography - mass spectrometry/mass spectrometry (LC-MS/MS) measurement and validation method.

This standard applies to rice, brown rice, corn, wheat, tea, mango juice concentrate, soy, apples, oranges, cabbage, green in Shanghai tralomethrin Determination of residues and confirmation.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.

Laboratory use specifications and test methods GB/T 6682 Analysis

3 Method summary

Sample remaining tralomethrin ethyl acetate (containing more fat sample with acetonitrile) extraction, and the extract after 37 °C or less concentrated Dover Rory silica column (containing more fat samples with a neutral alumina column, containing more pigment sample was added active carbon column) purification, performed using LC-MS/MS Qualitative and quantitative (external standard method).

4 Reagents and materials

Unless otherwise specified, the reagents were of analytical grade water as a water line with GB/T 6682 regulations.

4.1 ethyl acetate. chromatography.

4.2 acetonitrile. chromatography.

4.3 hexane. chromatographically pure.

4.4 acetone. chromatography.

4.5 sodium chloride.

4.6 anhydrous sodium. 650 °C burning 4h, cooled in a desiccator to room temperature and stored in a sealed bottle aside.

4.7 n-hexane - ethyl acetate (955) mixed solution. Take hexane 95mL, 5mL ethyl acetate was added, and mix.

4.8 n-hexane - ethyl acetate (6040) mixed solution. Take hexane 60mL, 40mL of ethyl acetate was added, and mix.

4.9 mobile phase. methanol -10mmol ammonium acetate (containing 0.1% formic acid) (8020, volume ratio).

4.10 Standard substances. tralomethrin (CAS Number. 66841-25-6), purity >=92%.

4.11 Standard substance stock solution. Weigh accurately take the right amount of reference material, dissolved in a small amount of acetone, and then adding the concentration of n-hexane dubbed 1mg/mL standard stock solution, and in the following -18 °C dark preservation, valid for 12 months.

Intermediate solution 4.12 Standard substance. standard required to take the above formulation stock solution was diluted with n-hexane at a concentration of 10µg/mL ~ 100µg/mL of the intermediate standard solution substance below -18 °C dark preservation, valid for three months.