GB/T 18932.17-2003Method for the determination of sixteen sulfonamides residues in honey -- LC-MS-MS method (English PDF)

Foreword

This Part of GB/T 18932 modifies and adopts Canadian standard ACC-056-V2.0

"Methods for the determination of sixteen sulfonamides residues in honey -

LC-MS-MS method". The main changes are as follow.

- ADJUST the test varieties;

- ADD the purified steps of benzene sulfonic acid cation exchange column and

Oasis HLB column;

- The liquid chromatogram's column and mobile phase are different;

- REPLACE single quadrupole mass detector with tandem quadrupole mass

detector.

Appendix A and Appendix B of this Part are informative.

This Part was proposed by Qinhuangdao Entry-Exit Inspection and Quarantine

Bureau of People's Republic of China.

This Part shall be under the jurisdiction of All China Federation of Supply and

Marketing Cooperatives.

Drafting organization of this Part. Qinhuangdao Entry-Exit Inspection and Quarantine

Bureau of People's Republic of China.

1 Scope

This Part of GB/T 18932 specifies the determination method of sixteen sulfonamides

residues in honey - LC-MS-MS method.

This Part applies to the determination of sixteen sulfonamides residues.

Sulfamethizole is 1.0µg/kg; N-((4-Aminophenyl)sulfonyl)acetamide, sulfadiazine,

sulfapyridine, sulfisoxazole, sulfamerazine, sulfachloropyridazine, sulfamonomethoxine,

sulfadoxine, sulfamethoxazole are 2.0 µg/kg respectively; sulfathiazole,

sulfamethoxypyridazine, sulfadimethoxypyrimidine are 4.0 µg/kg respectively;

sulfameter, sulfamethazine are 8.0 µg/kg respectively; sulfaphenazole is 12.0

µg/kg.

2 Normative references

The following documents contain provisions which, through reference in this Part,

become the provisions of this Part. For dated references, their subsequent

amendments (excluding corrections) or revisions do not apply to this Part. However,

the parties who enter into agreement based on this Part are encouraged to investigate

whether the latest versions of these documents are applicable. For undated reference

documents, the latest versions apply to this Part.

GB/T 6379 Precision of test methods - Determination of repeatability and

reproducibility for a standard test method by interlaboratory tests (GB/T 6379-1986,

neq ISO 5725.1981)

GB/T 6682 Water for analytical laboratory use - Specification and test methods

(GB/T 6682-1992, neq ISO 3696.1987)

3 Principle

Use phosphoric acid solution (pH=2) to extract the sulfonamides residues in honey;

leach the residues; purify through cation exchange column and Oasis HLB or

equivalent solid phase extraction column; use methanol to elute; evaporate and dry it;

use acetonitrile + ammonium acetate solution (0.1mol/L) to dissolve the residues. Use

GB/T 11064.8-2013

7 Determination steps

8 Calculation of results

The residues of each kind of sulfonamides in the samples are calculated by data

processing system or calculated according to equation (1).

1000--

VcX... (1)

Where,

X - the residues of the tested component in the sample, in micrograms per kilogram

(µg/kg);

c – concentration of the tested component solution, obtained from standard

working curve, in nanograms per milliliter (ng/mL);

V – the constant volume of sample solution, in milliliters (mL);

m – mass of the representative samples in sample solution, in grams (g).

Note. the blank values shall be deducted from the calculation results.

9 Precision

The precision data in this Part are determined in accordance with the specifications of

GB/T 6379. The repeatability and reproducibility values are calculated by 95%

confidence.

1 Sulfamethizole 144-82-1

2 N-((4-Aminophenyl)sulfonyl)acetamide 144-80-9

3 Sulfadiazine 68-35-9

4 Sulfapyridine 144-83-2

5 Sulfisoxazole 127-69-5

6 Sulfamerazine 127-79-7

7 Sulfachloropyridazine 80-32-0

8 Sulfamonomethoxine 1220-83-3

9 Sulfadoxine 2447-57-6

10 Sulfisoxazole 127-69-5

11 Sulfathiazole 72-14-0

12 Sulfamethoxypyridazine 80-35-3

13 Sulfadimethoxypyrimidine 155-91-9

14 Sulfamethazine 57-68-1

15 Sulfaphenazole 526-08-9

16 Sulfameter 651-06-9

......