GB/T 22966-2008Determination of sixteen sulfonamide 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. 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. Lv Hongying, paragraph Wenzhong, Chenrui Chun, Guo Chunhai, Yilian Feng, Gu Haitao, Doucai Yun, Mayu Song, Pang Guofang. Milk and milk powder 16 kinds of sulfa drug residues Determination of liquid chromatography - tandem mass spectrometry

1 Scope

GB/T 22966-2008 is the Chinese national standard on determination of sixteen sulfonamide 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 16 kinds of sulfonamides (see Table 2) residual amount of liquid chromatography - mass spectrometry/mass spectrometry. This standard applies to milk and milk powder Determination of 16 sulfonamides residues. The standard method detection limit. milk sulfacetamide, sulfamethyldiazine, sulfasalazine, sulfa methoxy pyridazine, sulfamethoxydiazine, Sulfa chlorine pyridazine, sulfamethoxazole Oxazole, o-methoxy pyrimidine sulfonamides, 6-methoxy pyrimidine sulfonamides, sulfamethazine, sulfaquinoxaline, sulfonamides Pyrimidine, Sulfathiazole, thiadiazole sulfamethoxazole, trimethoprim and sulfamethazine iso 16 kinds of sulfa drug residues detection method azoles Limits were 1.0µg/kg; milk powder sulfacetamide, sulfamethyldiazine, sulfasalazine, sulfa methoxy pyridazine, sulfamethoxydiazine, sulfa chlorine Pyridazine, sulfamethoxazole Oxazole, o-methoxy pyrimidine sulfonamides, 6-methoxy pyrimidine sulfonamides, sulfamethazine, quinoline sulfonamides, sulfadiazine, sulfonamide Amine thiazole, thiadiazole sulfamethoxazole, trimethoprim and sulfamethazine iso 16 kinds of sulfa drug residues method detection limits are azoles 4.0µg/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 Extracted with perchloric acid solution sample sulfa drug residues, OasisHLB SPE column 1) purification, methanol, liquid chromatography - mass Spectrum/mass spectrometer, external standard. 1) OasisHLB solid phase extraction columns are Waters company's product trade name, this information is given for the convenience of users of this standard, not the table Endorsement of the product shown. If other equivalent product has the same effect, you can use these equivalent products.

4 Reagents and materials

Unless otherwise stated, all reagents superior grade of pure water as a water GB/T 6682 regulations.

4.1 perchloric acid.

4.2 Methanol. chromatographically pure. Acetate 4.3. HPLC grade.

4.4 perchloric acid solution. pH = 2,1000mL 1mL perchloric acid in water was added, and then water was adjusted to pH = 2. 4.5 0.1% acetic acid solution. 100mL of water was added 0.1mL of acetic acid (4.3).

4.6 methanol - acetic acid solution (19 + 1). Measure 50mL methanol (4.2) (4.5) was mixed with 950mL acetic acid solution.

4.7 sulfacetamide, sulfamethyldiazine, sulfasalazine, sulfa methoxy pyridazine, sulfamethoxydiazine, sulfa chlorine pyridazine, sulfamethoxazole