SN/T 2453-2010Determination of zoalene residues in foodstuffs of animal origin for import and export. LC-MS/MS method (English PDF)

Foreword

The Standard Appendix A, Appendix B and Appendix C are informative appendices.

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

This standard by the People's Republic of China Heilongjiang Exit Inspection and Quarantine is responsible for drafting.

1 Scope

This standard specifies the sample preparation and liquid chromatography foods of animal origin dinitramide care amines - MS/MS detection and confirmation methods.

This standard applies to animal meat, liver, kidneys, milk dinitramide care amine residues determination.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequently Some amendments (not including errata content) or revisions do not apply to this standard, however, encourage the various aspects of the agreement in accordance with this standard Research using the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.

Laboratory use specifications and test methods GB/T 6682 Analysis

3 Method summary

The sample was extracted with acetonitrile dinitramide care amine extract was neutral alumina solid phase extraction (SPE), after the eluent volume was concentrated, liquid color Spectrum - mass spectrometry/mass spectrometer, external standard.

4 Reagents and materials

All reagents unless otherwise specified, the reagents were of analytical grade water as a water GB/T 6682 regulations.

4.1 acetonitrile. chromatography.

4.2 dichloromethane.

4.3 methanol.

4.4 acetone.

4.5 sodium chloride.

4.6 anhydrous sodium sulfate. After burning 650 °C 4h, cooled storage backup in a desiccator.

4.7 anhydrous sodium sulfate column. with an inner diameter of about 1.5cm lower portion of the glass tube shut up, shut at filling a small amount of glass wool and packed in dry sulfur Sodium, height of about 1.5cm.

4.8 methylene chloride - acetone (7 + 3) solution. Measure 100mL of acetone, diluted with 400mL dichloromethane.

4.9 methanol - acetone (8 + 2) solution. Measure 100mL of methanol, diluted with 400mL of acetone.

4.10 acetonitrile - water (4 + 6) was. Measure 400mL acetonitrile, diluted with water to 1000mL, through 0.22µm microporous membrane.

4.11 acetonitrile saturated n-hexane solution. 20mL of acetonitrile was added 100mL of n-hexane, followed by sufficient shaking, standing layer, the upper layer n-hexyl Chloride layer alternate.

4.12 neutral alumina SPE. 1000mg, 6mL, or equivalent person. 10mL of acetone were used before use, 10mL methylene Alkyl - acetone (7 + 3) pretreatment solution, and kept moist cylinder.

Note. neutral alumina SPE should be kept dry after opening.

4.13 Standard substances. dinitramide care amine purity of greater than 98.0%, C8H7N3O5, CAS. 148-01-6.

4.14 standard stock solution. Weigh accurately translated its purity was 100% by mass of dinitramide care amine standard 0.010g, dissolved in acetonitrile and Constant volume to 100mL, concentration equivalent to 100µg/mL. Stock solution at 0 °C ~ 4 °C refrigerator protected from light, can be used for six months.

4.15 intermediate standard solution. take the exact amount of standard stock solution 1.0mL, acetonitrile - was dissolved in water (4 + 6) and set the volume to 100mL, conc.