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GB 29696-2013 English PDF

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GB 29696-2013: Determination of Avermectin residues in milk by High Performance Liquid Chromatographic method
Status: Valid

Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
GB 29696-2013	English	229	Add to Cart	3 days [Need to translate]	Determination of Avermectin residues in milk by High Performance Liquid Chromatographic method	Valid	GB 29696-2013

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Basic data

Standard ID	GB 29696-2013 (GB29696-2013)
Description (Translated English)	Determination of Avermectin residues in milk by High Performance Liquid Chromatographic method
Sector / Industry	National Standard
Classification of Chinese Standard	C53
Classification of International Standard	67.020
Word Count Estimation	10,167
Quoted Standard	GB/T 6682; GB/T 1.1-2000
Adopted Standard	GB/T 6682; GB/T 1.1-2000
Regulation (derived from)	China Food & Drug Administration [2013] No. 234, November, 1, 2013
Issuing agency(ies)	Ministry of Agriculture of the People's Republic of China, National Health and Family Planning Commission of the People's Republic of China
Summary	This standard specifies the Milk avermectin Residues sample preparation method and HPLC.

GB 29696-2013: Determination of Avermectin residues in milk by High Performance Liquid Chromatographic method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of Avermectins residues in milk by High Performance Liquid Chromatographic method National Standards of People's Republic of China National Food Safety Standard Determination of residues in milk avermectin High performance liquid chromatography Published 2013-09-16 2014-01-01 implementation Ministry of Agriculture, People's Republic of China National Health and Family Planning Commission People's Republic of China released National Food Safety Standard Determination of residues in milk avermectin High performance liquid chromatography

1 Scope

This standard specifies the sample preparation and high performance liquid chromatographic method avermectin milk residues detected. This standard applies to the residual amount of ivermectin, abamectin, doramectin, and Eprinomectin single or multiple drugs in milk Detection.

2 Normative references

The following documents for the application of this document is essential. For dated references, only applies to the version dated paper Pieces. For undated references, the latest edition (including any amendments) applies to this document. GB/T 6682 Water for analytical laboratory specifications and test methods Principle 3 Avermectins in a sample drug residue, extracted with acetonitrile, C18 column purification, trifluoroacetic anhydride and N- methylimidazole derivatization, high performance liquid Phase Chromatography - Fluorescence method, external standard.

4 Reagents and materials

The following reagents used, unless otherwise stated are analytical reagents, water as a water line with GB/T 6682 provisions. 4.1 Eprinomectin, avermectin, ivermectin Standard. content ≥98%; doramectin Standard. content ≥94.3%. 4.2 Methanol. HPLC grade. 4.3 Acetonitrile. chromatographically pure. 4.4 trifluoroacetic anhydride. 4.5 triethylamine. 4.6 iso-octane. 4.7 N- methylimidazole. 4.8 C18 solid phase extraction column. 500mg/6mL, or equivalent person. 4.9 washing solution. Take acetonitrile 30mL, 70mL water and triethylamine 20μL, mix. 4.10 derivatizing agent solution A. N- methyl imidazole take 1mL, acetonitrile 1mL, mix, now with the current. 4.11 derivatization reagent B solution. Take trifluoroacetic anhydride 1mL, acetonitrile 2mL, mix, now with the current. 4.12 200μg/mL avermectin mixed standard stock solution. Weigh accurately Eprinomectin, avermectin, doramectin and Ibn Ivermectin 10mg of each standard in 50mL volumetric flask, dissolved in acetonitrile and dilute to volume, formulated at a concentration of 200μg/mL avermectins Cephalosporins drugs mixed standard stock solution. 2 ℃ ~ 8 ℃ or less, valid for 6 months. 4.13 10μg/mL avermectin working standard solutions. precise amount of 200μg/mL standard mixture of avermectin reservoir 0.5 mL was prepared, in 10mL volumetric flask, dissolved in acetonitrile and dilute to volume, avermectin formulation at a concentration of 10μg/mL of Standard working solution. 2 ℃ ~ 8 ℃ or less, valid for 6 months. 5. Apparatus 5.1 HPLC. with a fluorescence detector. 5.2 Analytical balance. a sense of volume 0.00001g. 5.3 Balance. a sense of the amount of 0.01g. 5.4 vortex mixers. 5.5 centrifuge. 5.6 SPE. 5.7 Nitrogen blowing instrument. 5.8 microporous membrane. 0.45μm. Preparation and Storage of sample 6 6.1 Preparation of the sample Fresh or thawed take appropriate blank or test milk and mix well. --- the test sample taken after homogenization, as the feed try. --- blank sample taken after homogenization, as a blank sample. --- blank sample taken after homogenization, adding a suitable concentration of the standard working, is added as a blank sample. Save 6.2 sample Or less at -20 ℃. Determination Step 7 7.1 Preparation of standard curve The precise amount of 10μg/mL avermectin amount mixed standard stock solution, diluted with acetonitrile, formulated at a concentration of 2,5,10,50, 100, 500 and 1000ng/mL standard solution series, depicting in 5mL 1.0mL tubes, at at 60 ℃ dry nitrogen, was added sequentially A 100μL derivatizing agent solution and 150 L of Solution B derivatizing reagents, sealed, vortexed 10s, glacial acetic acid and triethylamine were successively added 50 L each, Eddy 10s, with the sample solution synchronous closed reaction 30min, add 650μL of methanol mix for HPLC assay. To the measured peak area The vertical axis, corresponding to the concentration of standard solution as abscissa, the standard curve. Seeking regression equation and correlation coefficient. 7.2 extract Sample Weigh 5g ± 0.05g in 50mL centrifuge tubes, was added 8 mL of acetonitrile, vortexed 1min, 4500r/min centrifugal 10min, the Supernatant. The residue in 8 mL of acetonitrile was added, extraction was repeated once, the two supernatants were combined, water 20mL, 50 L of triethylamine, mixed and set aside. 7.3 Purification C18 column eluted sequentially with acetonitrile and the washing solution 5mL 5mL activation, taking stock solution through the column, the natural flow of dry, drained 5min, add 3mL isooctane Washed, drained 5min, 5mL acetonitrile, collecting eluate in 10mL tubes, blown dry with nitrogen at 60 ℃ at standby. 7.4 Derivatization Alternate tube in the added sequentially derivatizing agent solution A 100 L, 150 L of Solution B derivatizing reagents, sealed, vortexed 10s, sequentially ice 50 L of acetic acid and triethylamine 50μL, whirl 10s, closed reaction at room temperature for 30min, add 650μL of methanol and mix. Filtration, high performance liquid supply Phase Chromatography. 7.5 Determination 7.5.1 LC reference condition 7.5.1.1 Column. SymmetryC18 (250mm × 4.6mm, particle size 5μm), or equivalent person. 7.5.1.2 Mobile phase. aqueous acetonitrile (90 10, volume ratio). 7.5.1.3 flow rate. 1mL/min. 7.5.1.4 Column temperature. 30 ℃. 7.5.1.5 excitation wavelength. 365nm. 7.5.1.6 emission wavelength. 475nm. 7.5.1.7 Injection volume. 20μL. 7.5.2 Assay Take a sample solution and standard solutions corresponding, for single or multi-point calibration, by external standard method, the peak area is calculated. Standard solution and sample solution Avermectin broth response value should be within the linear range of the detection instrument. In the chromatographic conditions, the standard solution and blank add HPLC chromatograms of the sample solution in Appendix A. 7.6 Blank test But without addition of the sample, the same steps employed in parallel operation.

8 and the result of the calculation expression

Residue (μg/kg) in a sample of avermectin according to formula (1). X = c × V (1) Where. --- for X-amount of residual feed try avermectins corresponding drug, in micrograms per kilogram (μg/kg); --- C concentration in the sample solution corresponding avermectin, in units of micrograms per milliliter (μg/mL); V --- total volume of the sample solution, in milliliters (mL); m --- try supply feed mass in grams (g). Note. The blank value should be subtracted from the results, expressed as the arithmetic mean of the measurement result measured parallel to three significant figures. 9 detection sensitivity, accuracy and precision 9.1 Sensitivity The detection limit of the method was 1μg/kg, the limit of quantitation of 2μg/kg. 9.2 Accuracy This method of adding 2μg/kg ~ 100μg/kg on recovery levels of 70% to 120%. 9.3 Precision The relative standard deviation of the method ≤15%, inter-assay relative standard deviation ≤20%.

Appendix A

Chromatogram Description. 1 --- Eprinomectin; 2 --- avermectin; 3 --- doramectin; 4 --- ivermectin. a) avermectin chromatogram of the standard solution (10ng/mL) Description. 1 --- Eprinomectin; 2 --- avermectin; 3 --- doramectin; 4 --- ivermectin. b) adding milk avermectin blank sample chromatogram (2μg/kg) c) a blank sample chromatogram milk Figure A.1 chromatogram

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