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Determination of streptomycin residues in royal jelly and royal jelly powder for import and export. Liquid chromatographic method
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Basic data | Standard ID | SN/T 1775-2006 (SN/T1775-2006) | | Description (Translated English) | Determination of streptomycin residues in royal jelly and royal jelly powder for import and export. Liquid chromatographic method | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | B47;X31 | | Classification of International Standard | 67.180.10 | | Word Count Estimation | 14,180 | | Date of Issue | 2006-04-25 | | Date of Implementation | 2006-11-15 | | Regulation (derived from) | Industry Standard Notice 2006 No. 7 (No. 79 overall) | | Issuing agency(ies) | General Administration of Customs | | Summary | This standard specifies the import and export of royal jelly and royal jelly lyophilized streptomycin residues in sample preparation and liquid chromatographic method. This standard applies to imports and royal jelly and royal jelly lyophilized streptomycin residues detected. | SN/T 1775-2006: Determination of streptomycin residues in royal jelly and royal jelly powder for import and export. Liquid chromatographic method
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Determination of streptomycin residues in royal jelly and royal jelly powder for import and export.Liquid chromatographic method
Book of the People's Republic of China Entry and Exit Inspection and Quarantine
Import and export of royal jelly and royal jelly lyophilized powder streptomycin
Residue detection method liquid chromatography
Released on.2006-04-25
Implementation of.2006-11-15
People's Republic
The General Administration of Quality Supervision, Inspection and Quarantine issued
Foreword
Appendix A of this standard is an informative annex.
This standard is proposed and managed by the National Certification and Accreditation Administration.
This standard was drafted. Zhejiang Entry-Exit Inspection and Quarantine Bureau of the People's Republic of China.
The main drafters of this standard. Chen Xiaomei, Chi Haochao, Chen Xiaoxia, Wang Dong, Shi Xuxia, Liu Haishan, Shi Lei.
This standard is the first industry standard for entry-exit inspection and quarantine.
Import and export of royal jelly and royal jelly lyophilized powder streptomycin
Residue detection method liquid chromatography
1 Scope
This standard specifies the preparation of samples for the detection of streptomycin residues in the royal jelly of imported and exported royal jelly and royal jelly, and the method for determination of liquid chromatography.
This standard applies to the detection of streptomycin residues in the import and export royal jelly and royal jelly lyophilized powder.
2 sample preparation
2.1 Preparation of samples
The sample to be extracted is thoroughly mixed and divided into two parts, which are respectively placed in a clean container, one is stored as a sample and the other is used as a sample.
For testing purposes. Samples should be protected from contamination or changes in content during sampling and sample preparation operations.
2.2 Storage of samples
The sample should be tested in time. If it cannot be detected in time, it should be stored frozen below -18 °C.
3 Determination method
3.1 Method summary
The streptomycin in the sample is extracted with dilute phosphoric acid, and the protein in the sample is precipitated by trichloroacetic acid. The supernatant is passed through the cation exchange column and the HLB solid phase.
Extraction cartridge purification. The streptomycin in the sample was determined by a liquid chromatography post-column fluorescence detector and quantified by external standard method.
3.2 Reagents and materials
Unless otherwise specified, the reagents were of analytical grade and the water was either distilled or deionized water.
3.2.1 Methanol. Liquid chromatography grade reagent.
3.2.2 Acetonitrile. liquid chromatography grade reagent.
3.2.3 Phosphoric acid. ≥ 85%.
3.2.4 Acetic acid.
3.2.5 Dipotassium hydrogen phosphate.
3.2.6 Potassium dihydrogen phosphate.
3.2.7 Sodium hydroxide.
3.2.8 Trichloroacetic acid.
3.2.9 Sodium heptane sulfonate (C7H15NaO3S.H2O). pure by liquid chromatography.
3.2.10 1,2-naphthoquinone-4-sulfonic acid sodium.
3.2.11 30% aqueous methanol. methanol + water (30 + 70, 犞/犞).
3.2.12 Dilute phosphoric acid solution. pH=2. Phosphoric acid was added dropwise to 1000 mL of water, and the pH of the solution was adjusted to 2 on a pH meter.
3.2.13 phosphate buffer solution. 0.2 mol/L, pH = 8. Weigh 33.46g dipotassium hydrogen phosphate and 1.05g potassium dihydrogen phosphate in a beaker
In the middle, add water to dissolve and dilute to 1000mL. The pH of the solution was adjusted to 8 with phosphoric acid.
3.2.14 sodium hydroxide solution. 0.2mol/L, weigh 8g of sodium hydroxide dissolved in an appropriate amount of water, and then make up to 1000mL.
3.2.15 Trichloroacetic acid solution. 50% aqueous solution. Weigh 100g of trichloroacetic acid dissolved in an appropriate amount of water, and then make up to 100mL.
3.2.16 Saturated sodium hydroxide solution.
3.2.17 Sodium heptanesulfonate solution. 0.5 mol/L, and 11 g of sodium heptanesulfonate was weighed and dissolved in 100 mL of water.
3.2.18 Heptanesulfonic acid sodium acid solution. 0.01 mol/L, pH 3.3. Weigh 2.2g of sodium heptane sulfonate dissolved in 900mL of water, add B
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