GB/T 22978-2008Determination of dexamethasone residues in milk and milk powder - LC-MS-MS method (English PDF)

Foreword

The Standard Appendix A, Appendix B is an informative annex. This standard is proposed and managed by the State Administration of Quality Supervision Inspection and Quarantine of People's Republic of China. This standard was drafted. People's Republic of China Exit Inspection and Quarantine Qinhuangdao, Hebei People's Republic of China Entry-Exit Inspection and Quarantine Bureau. The main drafters of this standard. Mayu Song, Gena, Guo Chunhai, paragraph Wenzhong, Chenrui Chun, Lv Hongying, Doucai Yun, Jia Haitao, Pang Guofang. Determination of milk and milk powder dexamethasone residues Liquid chromatography - tandem mass spectrometry

1 Scope

GB/T 22978-2008 is the Chinese national standard on determination of dexamethasone residues in milk and milk powder - lc-ms-ms method. The /T suffix marks it as a recommended standard: it is not compulsory by itself, but it becomes binding as soon as a contract, a tender or a customer specification calls it up - which in practice is how most foreign buyers meet it. It was issued on 31 December 2008 by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of China, and has been in force since 1 May 2009. Classification: ICS (ICS) , CCS X04. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

This standard specifies the milk and milk powder dexamethasone residues in liquid chromatography - tandem mass spectrometry. This standard applies to the determination of milk and milk powder dexamethasone residues and confirmation. The standard method detection limit. milk 0.2µg/kg, milk was 1.0µg/kg.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.

GB/T 6379.1 measurement methods and results of Accuracy (trueness and precision) - Part 1. General principles and definitions ( GB/T 6379.1-2004, ISO 5725-1.1994, IDT)

GB/T 6379.2 measurement methods and results of Accuracy (trueness and precision) - Part 2. Determine the standard measurement method to repeat Of the basic methods of reproduction ( GB/T 6379.2-2004, ISO 5725-2.1994, IDT)

GB/T 6682 analytical laboratory use specifications and test methods ( GB/T 6682-2008,

ISO 3696. 1987, MOD) Principle

3 Milk and milk samples were extracted with acetonitrile samples, C18 solid-phase extraction (SPE), liquid chromatography - tandem mass spectrometer, external standard.

4 Reagents and materials

Water as a water GB/T 6682 regulations.

4.1 Methanol. chromatographically pure.

4.2 acetonitrile. chromatography.

4.3 formic acid. pure class distinctions. 4.4 0.1% formic acid solution. Pipette 1mL acid (4.3) in 1L of water containing about 800mL flask with water to volume and mix. Dexamethasone

4.5 standard substance (CAS. 50-05-2). not less than 99% purity. Dexamethasone

4.6 standard stock solution. Weigh accurately 100mg dexamethasone standard substance (4.5), dissolved in methanol and set the volume to 100mL, dubbed the concentration of standard solution 1.0mg/mL of. The solution was stored at 4 °C. Dexamethasone

4.7 standard solution. draw the right amount of dexamethasone standard stock solution (4.6) with methanol dubbed 1µg/mL and 0.1µg/mL standard solution of two concentrations. The solution was stored at 4 °C.

4.8 dexamethasone matrix standard solution. draw the right amount of dexamethasone standard solution (4.7) as required, and extracted with a blank sample It was diluted to the appropriate concentration of the matrix standard working solution, prepared before use.

4.9 C18 solid phase extraction column. 500mg, 3mL. Before use, respectively 3mL 3mL of acetonitrile and water pretreatment column kept moist.

4.10 filter. 0.22µm.

5 Instruments and equipment

5.1 Liquid chromatography - tandem mass spectrometer. with atmospheric pressure chemical ionization (APCI).