Path: Home > GB > Page142 > GB 29703-2013

Price & Delivery

US$229.00 · In stock · Download in 9 seconds
GB 29703-2013: Determination of Sodium nifurstyrenate residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric 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

Std ID	Version	USD	Buy	Deliver [PDF] in	Title (Description)
GB 29703-2013	English	229	Add to Cart	3 days [Need to translate]	Determination of Sodium nifurstyrenate residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method

GB 29703-2013: Determination of Sodium nifurstyrenate residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric 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 Sodium nifurstyrenate residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method National Standards of People's Republic of China National Food Safety Standard Furan-benzene sodium acid residues in food animals is Liquid chromatography - tandem mass spectrometry 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 Furan-benzene sodium acid residues in food animals is Liquid chromatography - tandem mass spectrometry

1 Scope

This standard specifies the animal food furan benzene acid sodium Residues sample preparation and liquid chromatography - tandem mass spectrometry. Muscle and liver tissue This standard applies to pigs and chickens furan residual amounts of benzene acid sodium 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 Residual benzene in a sample furanyl acid sodium, 0.5% formic acid - ethyl acetate extraction, solid-phase extraction (SPE), liquid chromatography - tandem mass spectrometry ESI positive ion mode measurement, 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 furanyl benzene sodium acid standard. content of ≥98.0%. 4.2 methanol. 4.3 n-hexane. 4.4 Acetonitrile. chromatographically pure. 4.5 ethyl acetate. 4.6 formic acid. 4.7 HLB solid phase extraction column. 60mg/3mL, or equivalent person. 4.8 0.5% formic acid solution. Take acid 0.5mL, dissolve and dilute to 100mL with water. 4.9 0.5% formic acid - ethyl acetate solution. Take 200 mL of ethyl acetate, 0.5% formic acid solution was added 10mL, mix, now with the current. 4.10 1mg/mL sodium furan benzene acid standard stock solution. Weigh accurately furan-benzene standard acid sodium 10mg, in 10mL flask, Dissolved in dimethyl sulfoxide and diluted to the mark, formulated at a concentration of 1mg/mL of benzene, furan, sodium acid standard stock solution. -20 ℃ save less, Valid for six months. 4.11 10μg/mL sodium acid benzyl furan-standard working solution. precise amount of 1mg/mL sodium furan benzene acid standard stock solution 1.0mL, in 100mL volumetric flask, dissolved in mobile phase and dilute to volume, formulated at a concentration of 10μg/furan benzene acid sodium working standard solutions mL. -20 ℃ below, valid for six months. 5. Apparatus 5.1 liquid chromatography - tandem mass spectrometry. electrospray ionization with (ESI). 5.2 Analytical balance. a sense of volume 0.00001g. 5.3 Balance. a sense of the amount of 0.01g. 5.4 freezing high-speed centrifuge. 5.5 oscillator. 5.6 vortex mixer. 5.7 homogenizer. 5.8 Nitrogen blowing instrument. 5.9 rotary evaporator. 5.10 centrifuge tube. 50mL. 5.11 eggplant-shaped bottle. 5.12 filter. 0.22μm. Preparation and Storage of sample 6 6.1 Preparation of the sample Fresh or frozen blank or test tissue, minced, and homogenized. --- the test sample taken after homogenization, as the test material. --- blank sample taken after homogenization, as a blank material. --- blank sample taken after homogenization, adding a suitable concentration of the standard working solution, is added as a blank sample. Save 6.2 sample Or less at -20 ℃. Determination Step 7 7.1 extract Take Sample 2g ± 0.05g, in 50mL centrifuge tubes, add 0.5% formic acid - ethyl acetate solution 15mL, vortexed, shaken 5min, 8000r/min centrifugal 10min, the ethyl acetate layer eggplant-shaped flask, the residue was added 0.5% formic acid - ethyl acetate solution 10mL, heavy Re-extracted once, twice with ethyl acetate layers were combined, rotary evaporated at 45 ℃ to dryness, treated with 50% aqueous acetonitrile and the residue was dissolved 3mL, go Centrifuge tube with 3mL washed with 50% aqueous acetonitrile eggplant-shaped flask, two washings were combined, hexane was added 3mL, shaking after mixing, 5000r/min centrifugal 5min, the lower layer was taken and set aside. 7.2 Purification HLB column eluted sequentially with methanol and 3mL 3mL water activation, taking stock solution through the column. 6mL water rinsed, drained, washed 3mL of acetonitrile was added Off, the eluate was collected, dried under nitrogen 50 ℃, the mobile phase the residue was dissolved 1.0mL, 1.5mL transferred to centrifuge tube, 10000r/min Centrifugal 10min, supernatant, membrane filtration, liquid chromatography - tandem mass spectrometry. 7.3 Preparation of standard curve They were the precise amount of 10μg/mL sodium acid benzyl furan-standard working fluid amount, diluted with mobile phase to prepare a concentration of 0.2,0.5,2, 5 and 8μg/L series of standard solutions, the liquid chromatography - tandem mass spectrometry. A characteristic ion mass chromatogram peak area for the vertical axis, standard solutions Concentration as the abscissa, the standard curve. 7.4 Determination 7.4.1 LC Conditions 7.4.1.1 Column. C18 (150mm × 2.1mm, particle size 5μm), or equivalent person. 7.4.1.2 Mobile phase. aqueous acetonitrile (40 60, volume ratio). 7.4.1.3 Column temperature. 40 ℃. 7.4.1.4 Injection volume. 10μL. 7.4.2 MS conditions 7.4.2.1 ion source. electrospray ionization source. 7.4.2.2 Scan mode. positive ion scan. 7.4.2.3 Detection mode. selective reaction monitoring. 7.4.2.4 Spray voltage. 4000V. 7.4.2.5 Ion transfer tube temperature. 330 ℃. 7.4.2.6 Sheath Gas Pressure. 40arb. 7.4.2.7 Auxiliary gas pressure. 6arb. 7.4.2.8 optimization parameters selected reaction monitoring. Table 1. Table 1 Sodium Benzene furanyl acid selected reaction monitoring of optimization parameters Drug Name Relative retention time min Qualitative ion pair m/z Quantitative ion pair m/z Collision energy eV Furan benzene acid 6.5 Sodium 290.18 > 202.43 290.18 > 228.26 290.18 > 228.26 7.4.3 Assay Take a sample and standard solutions, multi-point calibration is calculated, the external standard method. The sample solution and the standard solution of sodium acid benzyl furan-average peak area It should be in the linear range of the detection instrument. Ion in the sample solution as compared to the relative abundance of the standard relative abundance of ions in solution, in line with Table 2 is required. Added standard solution and blank sample solution ion mass chromatogram characteristic Appendix A. The maximum allowable deviation relative ion abundance qualitative determination of Table 2 The relative ion abundances > 50 20 ~ 50 10 ~ 20 ≤10 Permissible relative deviation ± 20 ± 25 ± 30 ± 50 7.5 Blank test But without addition of the sample, the same steps employed in parallel operation. Calculation and Expression of Results 8 From a standard curve calibrated by. AS = acS b to obtain a and b, then c = (Ab)/a (1) Residues in the specimens furan benzene acid sodium (μg/kg) according to formula (2). X = A × cS × V AS × m (2) Where. --- the AS acid in a standard solution of sodium benzene furan-peak area; Furan benzene concentration of sodium cS --- acid standard solution, units of nanograms per milliliter (ng/mL); A --- furan sample solution of sodium benzene acid peak area; --- the specimens residues X-furanyl benzene sodium acid micrograms per kilogram (μg/kg); V --- The residue was dissolved in mobile phase volume 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 0.2μg/kg, the limit of quantitation was 0.5μg/kg. 9.2 Accuracy This method of adding 0.5μg/kg ~ 2μg/kg on recovery levels of 60% to 120%. 9.3 Precision ≤20% relative standard deviation in this method and inter - batch relative standard deviation of ≤25%.

Appendix A

Chromatogram Figure A.1 furan benzene acid sodium ion chromatogram of the standard solution (0.5μg/L) Figure A.2 pig liver tissue sample blank ion chromatogram Figure A.3 blank add pig liver tissue sample furan benzene acid sodium ion chromatogram (0.5μg/kg) ...