GB/T 22960-2008Determination of cefazolin, cefapirin, cephalexin, cefalonium, cefquinome residues in fugu and 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. Li Xuemin, Wang Heqin, female health, Caoyan Zhong, FEDERATION Pang Guofang. Puffer fish and eel cefazolin, cephalosporins aspirin, Cephalexin, CTP, cefquinome Determination of residues of liquid chromatography - tandem mass spectrometry

1 Scope

GB/T 22960-2008 is the Chinese national standard on determination of cefazolin, cefapirin, cephalexin, cefalonium, cefquinome residues in fugu and 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: 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 and eel cefazolin, cephalosporins, aspirin, cephalexin, CTP, cefquinome residues in liquid chromatography Spectrum - tandem mass spectrometry. This standard applies to puffer fish and eel cefazolin, cephalosporins, aspirin, cephalexin, CTP, cefquinome residues determination. The standard method detection limit. cefazolin is 10µg/kg; cephalosporin aspirin, cephalexin, CTP, cefquinome is 2.0µg/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 Sample of Five cephalosporin drug residues were extracted with acetonitrile, acetonitrile was removed by rotary evaporation, water volume, liquid chromatography - tandem mass spectrometer Fixed, external standard.

4 Reagents and materials

Unless otherwise indicated, the reagents used were of analytical grade.

4.1 Water. GB/T 6682, level.

4.2 Methanol. chromatographically pure.

4.3 acetonitrile. chromatography.

4.4 acetic acid.

4.6 acetonitrile saturated with n-hexane. Take 100mL n-hexane (4.5) and 50mL of acetonitrile (4.3) in the 250mL separating funnel, shaken 1min, After standing layer discarded acetonitrile.

4.7 Standard substance. cefazolin (CAS. 25953-19-9), cephalosporin aspirin (CAS. 24356-60-3), cephalexin (CAS. 16549-56-7), Cephalosporins Luoning (CAS. 5575-21-3), cefquinome (CAS. 118443-89-3), purity >=99%. 4.8 1.0mg/mL five kinds of cephalosporin standard stock solution. Weigh accurately take the right amount of each standard substance (4.7), were formulated into water Concentration of 1.0mg/mL of the standard stock solution. Stock solution stored at -18 °C freezer.

4.9 five kinds of mixed standard working solution cephalosporins. cephalosporin draw the right amount of each standard stock solution (4.8) if necessary, dilute with water Release an appropriate concentration of the mixed standard working solution.