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GB/T 22988-2008: Determination of spiramycin, pirlimycin, oleandomycin, tilmicosin, erythromycin and tylosin residues in milk and milk powder - LC-MS-MS method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 22988-2008: Determination of spiramycin, pirlimycin, oleandomycin, tilmicosin, erythromycin and tylosin residues in milk and milk powder - LC-MS-MS method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT22988-2008 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 67.050 X 04 Determination of spiramycin, pirlimycin, oleandomycin, tilmicosin, erythromycin and tylosin residues in milk and milk powder - LC-MS-MS method ISSUED ON: DECEMBER 31, 2008 IMPLEMENTED ON: MAY 01, 2009 Issued by: General Administration of Quality Supervision, Inspection and Quarantine of PRC; National Standardization Administration. Table of ContentsForeword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Principle ... 5 4 Reagents and materials ... 5 5 Instruments and equipment ... 6 6 Preparation and storage of specimens ... 6 7 Determination steps ... 6 8 Result calculation ... 10 9 Precision ... 10 Appendix A (Informative) Multiple reaction monitoring (MRM) chromatograms of standard substances ... 12 Appendix B (Informative) Recovery ... 13 Determination of spiramycin, pirlimycin, oleandomycin, tilmicosin, erythromycin and tylosin residues in milk and milk powder - LC-MS-MS method1 ScopeThis standard specifies the HPLC-tandem mass spectrometry method for the determination of spiramycin, pirlimycin, oleandomycin, tilmicascin, erythromycin, tylosin residues in milk and milk powder. This standard is applicable to the determination and confirmation of spiramycin, pirlimycin, oleandomycin, tilmicascin, erythromycin, tylosin residues in milk and milk powder. The method detection limit of this standard is 1 μg/kg for milk and 8 μg/kg for milk powder.2 Normative referencesThe clauses in the following documents become the clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding corrections) or revisions are not applicable to this standard. However, parties that reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version applies to this standard. GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725- 1:1994, IDT) GB/T 6379.2 Measurement methods and results - Accuracy (trueness and precision) - Part 2: Determine the standard methods of measurement repeatability and reproducibility of the basic method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT) GB/T 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)3 PrincipleThe analytes in the specimen are extracted with acetonitrile, cleaned up with solid phase extraction column, determined by high performance liquid chromatography-tandem mass spectrometry, quantified by external standard method.4 Reagents and materialsUnless otherwise specified, all reagents used are analytical grade; the water is grade 1 water as specified in GB/T 6682. 4.1 Acetonitrile, HPLC grade. 4.2 Methanol, HPLC grade. 4.3 Acetic acid, HPLC grade. 4.4 Ammonium formate, HPLC grade. 4.5 Disodium hydrogen phosphate. 4.6 Sodium hydroxide. 4.7 Methanol-water solution (3 + 7): 300 mL of methanol mixed with 700 mL of water. 4.8 5 mol/L sodium hydroxide solution: Weigh 20 g of sodium hydroxide; dissolve it in water; dilute it to 100 mL. 4.9 0.1 mol/L phosphate buffer solution: Dissolve 6 g of disodium hydrogen phosphate (4.5) in 450 mL of water; use sodium hydroxide (4.8) solution to adjust pH to 8; add water to 500 mL; prepare it before use. 4.10 0.1 mol/L ammonium formate solution: Add water to dissolve 0.63 g of ammonium formate (4.4) to 1000 mL. 4.11 Standard products: Spiramycin (CAS: 8025-81-8), pirlimycin (CAS: 79548-73-5), oleandomycin (CAS: 7060-74-4), tilmicosin (CAS: 108050-54-0), erythromycin (CAS: 114-07-8), tylosin (CAS: 1401-69-0), purity greater than or equal to 98%. 4.12 Standard stock solution: Accurately weigh appropriate amount of standard products; use methanol to prepare 100 μg/mL standard stock solution. 4.13 Mixed standard intermediate working solution: Take 1 mL of each standard stock solution (4.12) into a 100 mL volumetric flask; use methanol to dilute to the mark; prepare a mixed standard working solution which has a concentration of 1 μg/mL. 10 mL of acetonitrile to repeat extraction once. Combine the supernatant in the same chicken heart bottle. 7.1.2 Milk powder Weigh 0.5 g, accurate to 0.01 g, of the milk powder sample. Add 4 mL of water to a 50 mL stoppered centrifuge tube and mix well. Add 20 mL of acetonitrile. Oscillate for extraction for 2 min. Centrifuge at 3000 r/min for 10 min. Remove the supernatant and filter it into a chicken heart bottle. Use 10 mL of acetonitrile to repeat the extraction once. Combine the supernatant in the same chicken heart bottle. 7.2 Purification Rotate and evaporate the extract at 45 °C to about 4 mL. Add 2 mL of phosphate buffer (4.9). Mix well. Transfer to the conditioned HLB solid phase extraction column (4.15). Wash the chicken heart bottle twice with 2 mL of phosphate buffer. Transfer the washing liquid to the column. Drip it at a flow rate of less than 2 mL/min. Then, wash with 3 mL of water and 2 mL of methanol-water solution (4.7) in turn. Drain the column. Finally elute with 6 mL of acetonitrile and collect in a 10 mL graduated glass tube (the flow rate in this process is less than 2 mL/min). The eluent is blown to about 1 mL with nitrogen in a 45 °C water bath; use ammonium formate solution (4.10) to make its volume reach to 2 mL. After vortex mixing, filter it through a 0.45 µm filter membrane for HPLC-MS-MS analysis. 7.3 Preparation of blank matrix solution Take 4 g of milk negative sample and 0.5 g of milk powder negative sample, accurate to 0.01 g. Operate according to 7.1 and 7.2. 7.4 Determination conditions 7.4.1 Liquid chromatography reference conditions Liquid chromatography reference conditions are as follows: a) Chromatographic column: Phenyl column, 5 μm, 150 mm × 2.1 mm (inner diameter) or equivalent; b) Chromatographic column temperature: 30 °C; c) Injection volume: 15 μL; d) Mobile phase gradient and flow rate are shown in Table 1. can be found in Figure A.1 in Appendix A. 7.5 Parallel test According to the above steps, parallel test determination is carried out on the same specimen. 7.6 Recovery test Pipette an appropriate amount of mixed standard working solution. Use blank matrix solution to dilute it to the standard calibration solution of required concentration. Add standard solution to negative sample and operate according to 7.1 and 7.2. After determination, calculate the recovery of sample addition. The recovery range is shown in Table B.1 in Appendix B. 7.7 Blank test Follow the above steps except that the sample is not weighed.8 Result calculationThe residual amount of analyte in the specimen is calculated using the data processing system or according to formula (1): Where: Xi - The residual amount of the measured component in the specimen, in micrograms per kilogram (μg/kg); ci - The concentration of the measured component solution obtained from the standard working curve, in nanograms per milliliter (ng/mL); Vi - The final volume of the sample solution, in milliliters (mL); mi - The amount of the final sample represented by the sample solution, in grams (g). The blank value shall be deducted from the calculation result.9 Precision9.1 General provisions ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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