SN 0520-1996Determination of imazalil in cereals for export. HPLC-MS/MS method (English PDF)

Foreword

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

This standard replaces SN 0520-1996 "cereals for export ene bacteria residues in spirit." Compared with SN 0520-1996, in addition to editorial changes outside the main technical changes are as follows.

--- Change the standard name;

--- Liquid Chromatography - UV detection method is changed to liquid chromatography - mass spectrometry/mass spectrometry, lower detection limit;

--- Modify the pre-treatment methods.

Please note that some of the content of this document may involve patents. Release mechanism of the present document does not assume responsibility for the identification of these patents.

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

This standard was drafted. People's Republic of China Shanghai Entry-Exit Inspection and Quarantine Bureau, Xiamen People's Republic of China Entry-Exit Inspection and Quarantine Bureau.

1 Scope

This standard specifies the method for determination of cereals for export ene benomyl residues.

This standard applies to wheat, barley, rice, sorghum, maize, rice residues ene benomyl liquid chromatography - mass spectrometry/mass spectrometer.

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

Specimen under anhydrous sodium sulfate and sodium chloride salting, were extracted with acetonitrile, liquid chromatography and then by water dilution - mass spectrometry/mass spectrometer Fixed, external standard.

4 Reagents and materials

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

4.1 acetonitrile. high performance liquid chromatography.

4.2 anhydrous sodium sulfate. AR, 650 °C burning 4h, cooled storage in a closed container in the back.

4.3 sodium chloride.

4.4 formic acid. purity >=99%.

4.5 aqueous acetonitrile. water. acetonitrile (73, volume ratio).

4.6 0.1% formic acid solution. 1mL acid is dissolved in water and dilute to 1L.

4.7 Pesticide Standards. ene bacteria Ling (Imazalil, CAS number. 35554-44-0). purity >=98.0%.

4.8 preparation of standard stock solution. accurately weighed amount of ene benomyl standards, formulated as acetonitrile concentration of 1.0mg/mL standard Quasi stock solution. The solution was stored at -18 °C refrigerator for a period of 12 months.

Preparation 4.9 standard intermediate solution. diluted with acetonitrile standard stock solution to a final concentration of about 1.0µg/mL, less than 4 °C cold dark Tibetan save for a period of six months.

Preparation of standard solution of 4.10. necessary, standard intermediate solution absorb a certain amount of temporary use with aqueous acetonitrile (4.5) formulated as Appropriate concentrations of mixed standard working solution. Refrigerated below 4 °C dark, using now.

4.11 microporous membrane. 0.22µm, organic.

5 Instruments and equipment

5.1 Liquid chromatography - mass spectrometry/mass spectrometer. with electrospray ionization (ESI).