SN 0197-1993Method for determination of olaquindox metabolites residues in foodstuff of animal 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 0197-1993 "Olaquindox residues in meat exports." this standard compared with SN 0197-1993, the main technical changes are as follows.

--- Modify the standard Chinese name, standard Chinese name to "export food of animal origin in the determination of olaquindox metabolite residues Liquid Chromatography - Mass Spectrometry/Mass Spectrometry ";

--- Instrumentation changed from the original HPLC liquid chromatography - mass spectrometry/mass spectrometry;

--- Standards to extend the scope of the chicken food of animal origin pork, liver, eel, shrimp, beef;

--- Olaquindox to be detected by the identification of its metabolite 3-methyl quinoxaline-2-carboxylic acid;

--- Revised front portion of the sample processing steps and instruments measuring conditions;

--- Omitted sampling procedure.

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

This standard was drafted. China Inspection and Quarantine Science Research Institute, People's Republic of China Fujian Exit Inspection and Quarantine.

1 Scope

This standard specifies the determination of metabolite residues in food of animal origin export olaquindox.

This standard applies to pork, beef, chicken, fish, shrimp, liver and other foods of animal origin olaquindox metabolite 3-methyl-quinoxaline-2-carboxylic acid Determination (MQCA) residues.

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

Samples of 3-methyl-quinoxaline-2-carboxylic acid by hydrolysis, hydrochloric acid, hexane, and after centrifugation, the aqueous phase was mixed with a solution Co-type anion-exchange solid-phase extraction (SPE), liquid chromatography - mass spectrometry/mass spectrometer, internal standard.

4 Reagents and materials

Except where noted, all reagents were of analytical grade water as a water according to GB/T 6682 regulations.

4.1 acetonitrile. chromatography.

4.2 Methanol. chromatographically pure.

4.3 formic acid. Chromatographic pure.

4.4 ethyl acetate.

4.5 n-hexane.

4.6 of concentrated hydrochloric acid.

4.7 Aqueous ammonia (25% to 28% concentration).

4.8 acetic acid.

4.9 sodium acetate.

4.10 formic acid in ethyl acetate. 2%. 10mL 400mL ethyl acetate was added formic acid, ethyl acetate plus diluted to 500mL.

4.11 formic acid solution. 0.1%. 800mL of water was added 1.0mL of formic acid, add water to dilute 1L.

4.12 formic acid solution. 0.2%. 800mL of water was added 2.0mL of formic acid, add water to dilute 1L.

4.13 hydrochloric acid solution. 0.1mol/L. Pipette 8.3mL of concentrated hydrochloric acid, dissolved in water, dilute to 1L.

Hydrochloric acid solution 4.14; 0.3mol/L. Pipette 25mL of concentrated hydrochloric acid, dissolved in water, dilute to 1L.

4.15 Protease Protease. SigmaP5147 or equivalent below -18 °C preservation.

4.16 Protease solution. 0.01g/mL. Weigh 1.00gProtease protease (4.15), dissolved in water, dilute to 100mL, 4 °C save.