GB/T 22957-2008Determination of nine glucocorticoids residues in fugu, eel and baked eel - 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. This standard was drafted. People's Republic of China Qinhuangdao Exit Inspection and Quarantine. The main drafters of this standard. Liu Yongming, Li, Wu Yanping, Feng crown, Caoyan Zhong, Pang Guofang. Puffer fish, eel and eel of nine glucocorticoid Determination of residues Liquid chromatography - tandem mass spectrometry

1 Scope

GB/T 22957-2008 is the Chinese national standard on determination of nine glucocorticoids residues in fugu, eel and baked eel - 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 puffer fish, eel and eel prednisolone, prednisone, hydrocortisone, hydrocortisone, methylprednisolone, betamethasone Pine, dexamethasone, beclomethasone, fludrocortisone acetate, nine kinds of glucocorticoids residues in liquid chromatography - tandem mass spectrometry. This standard applies to fish, eel and eel of nine glucocorticoids residues measured puffer. The standard method detection limit. prednisolone, prednisone, hydrocortisone, hydrocortisone, methylprednisolone, betamethasone, dexamethasone Of 0.2µg/kg; beclomethasone, fludrocortisone acetate, 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 After the puffer fish, eels, eel sample was added anhydrous sodium sulfate, extracted with ethyl acetate extract was concentrated and subjected to silica gel solid phase extraction column Purification, liquid chromatography - tandem mass spectrometer, external standard.

4 Reagents and materials

4.1 Water. GB/T 6682, level.

4.2 Methanol. chromatographically pure.

4.3 acetonitrile. chromatography.

4.4 ethyl acetate. chromatography.

4.5 formic acid. pure class distinctions.

4.6 hexane. chromatographically pure.

4.7 acetone. chromatography.

4.8 acetone - n-hexane. acetone + hexane (3 + 2). Measure 200mL acetone and 300mL hexane mix.

4.9 anhydrous sodium. AR. Burning 6h at 650 °C muffle furnace and stored in a desiccator.

4.10 prednisolone (CAS. 50-24-8), prednisone (CAS. 53-03-2), hydrocortisone (CAS. 50-23-7), cortisone (CAS. 53- 06-5), methylprednisolone (CAS. 83-43-2), betamethasone (CAS. 378-44-9), dexamethasone (CAS. 50-02-2), beclomethasone (CAS. 4419-39-0), fludrocortisone acetate (CAS. 514-36-3) standard substance. purity >=98%. 4.11 1.0mg/mL standard stock solution. Weigh accurately take the right amount of each standard glucocorticoid substance, dissolved in methanol, were formulated as