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GB 29705-2013: Determination of Cypermethrin, Fenvalerate and Deltamethrin residues in aquatic products by Gas Chromatographic method
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Determination of Cypermethrin, Fenvalerate and Deltamethrin residues in aquatic products by Gas Chromatographic method
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GB 29705-2013
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Basic data
| Standard ID | GB 29705-2013 (GB29705-2013) |
| Description (Translated English) | Determination of Cypermethrin, Fenvalerate and Deltamethrin residues in aquatic products by Gas Chromatographic method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 10,168 |
| 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 Aquatic cypermethrin, fenvalerate, deltamethrin residues sample preparation and gas chromatographic method. |
GB 29705-2013: Determination of Cypermethrin, Fenvalerate and Deltamethrin residues in aquatic products by Gas 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 Cypermethrin, Fenvalerate and Deltamethrin residues in aquatic products by Gas Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Aquatic products cypermethrin, fenvalerate, deltamethrin
Multiresidue by gas 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
Aquatic products cypermethrin, fenvalerate, deltamethrin
Multiresidue by gas chromatography
1 Scope
This standard specifies the aquatic cypermethrin, fenvalerate and deltamethrin residues sample preparation and gas chromatographic method.
This standard applies to edible tissue of fish and shrimp detecting cypermethrin, fenvalerate and deltamethrin residues.
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
The specimens remaining cypermethrin, fenvalerate and deltamethrin, dehydrated with sodium chloride, extracted with acetonitrile, hexane degreasing, C18 column purification,
Determined by gas chromatography, external standard.
4 Reagents and materials
The following reagents used, unless otherwise stated were of analytical reagent; water as a water line with GB/T 6682 provisions.
4.1 cypermethrin, fenvalerate, deltamethrin standard. content ≥99.0%.
4.2 Acetonitrile. chromatographically pure.
4.3 Methanol. HPLC grade.
4.4 hexane. chromatography.
4.5 Benzene. chromatography.
4.6 ethyl acetate. chromatography.
4.7 chloroform. HPLC grade.
4.8 Sodium chloride. excellent pure, 650 ℃ burning 4h, cooled, dried and stored for use.
Aqueous methanol 4.9. Methanol 100mL, dissolved and diluted to 300mL with water.
4.10 n-hexane solution in acetonitrile. acetonitrile take 10mL, was dissolved with n-hexane and diluted to 110mL.
4.11 C18 solid phase extraction column.200mg/3mL, or equivalent person.
4.12 alumina SPE.200mg/3mL, or equivalent person.
4.13 100μg/mL cypermethrin, fenvalerate and deltamethrin standard stock solution. Weigh accurately cypermethrin, fenvalerate and bromine
Cyhalothrin each standard 10mg, brown in 100mL flask, dissolve and dilute benzene, formulated at a concentration of 100μg/mL of
Mixed standard stock solution. 2 ℃ ~ 8 ℃ storage period of three months.
4.14 5μg/mL cypermethrin, fenvalerate and deltamethrin working standard solutions. precise amount of 100μg/mL cypermethrin, pentyl cyanide
Permethrin and deltamethrin 500 L standard stock solution, brown in 10mL volumetric flask, dilute to the mark with benzene, formulated at a concentration of
5μg/mL of cypermethrin, fenvalerate and deltamethrin working standard solutions. 2 ℃ ~ 8 ℃ storage period of three months.
5. Apparatus
5.1 Gas chromatograph. 63Ni with an electron capture detector.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 homogenizer.
5.5 rotary evaporator.
5.6 centrifuge.
5.7 speed shaker.
5.8 Nitrogen blowing instrument.
5.9 SPE.
5.10 heart-shaped bottle. 125mL.
5.11 stoppered centrifuge tube. 10mL, 50mL.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Take appropriate blank or fresh or thawed fish and shrimp test edible tissue, minced, and homogenized.
--- 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 solution, is added as a blank sample.
Save 6.2 sample
Or less at -20 ℃.
Determination Step 7
7.1 extract
Sample Weigh 5g ± 0.05g, in 50mL glass centrifuge tube with stopper, acetonitrile was added 15mL, shaking 5min, sodium chloride 1.5g vibrator
Swing 2min, 4000r/min centrifugal 5min, supernatant to another glass stoppered centrifuge tube, the residue was added acetonitrile 15mL, extraction was repeated
Once, twice supernatants were combined, acetonitrile, n-hexane solution was added 10mL, shaking mixing 2min, 4000r/min centrifugal 5min, the upper layer was removed
Hexane solution, acetonitrile, n-hexane solution was added 10mL, extraction was repeated once, the upper n-hexane was discarded. The acetonitrile layer was taken to heart-shaped flask, to
45 ℃ water bath rotary evaporated to dryness, the residue was dissolved in methanol 2mL, 4 mL water was added, mixed and set aside.
7.2 purification and concentration
5mL C18 column successively with methanol, 5mL of chloroform, methanol and aqueous methanol 5mL 5mL activation, taking stock solution through the column, the control
Flow rate of 1 drop/s. 5mL rinsed with aqueous methanol, dried stream, Benzene was added 4mL, collecting eluate standby.
5mL activated alumina column with acetonitrile, the eluent through the column to take backup. Benzene was added 1mL elution, is repeated three times. Three eluent to merge
10mL graduated centrifuge tube, with the volume of benzene to 5mL, gas phase chromatography.
7.3 Preparation of standard curve
The precise amount of 5μg/mL cypermethrin, fenvalerate and deltamethrin amount standard stock solution, diluted with benzene, prepared to a concentration points
Do is a series hybrid standard 0.5,1,5,25,50,100 and 500ng/mL solution, gas phase chromatography. To the measured peak area for the vertical take
Standard, the standard concentration corresponding to abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 Chromatographic conditions
7.4.1.1 Detector. 63Ni electron capture detector.
7.4.1.2 Column. 5% phenyl and 95% polydimethylsiloxane.
7.4.1.3 Detector temperature. 310 ℃.
7.4.1.4 Inlet temperature. 230 ℃.
7.4.1.5 Injection mode. splitless.
7.4.1.6 Carrier gas. 99.999% pure nitrogen.
7.4.1.7 column flow rate. 2.5mL/min, the tail is blown. 25mL/min.
7.4.1.8 Column temperature program. initial column temperature 160 ℃, maintained 1min, 30 ℃/min was raised to 250 ℃, maintained 2min, 5 ℃/min was raised
280 ℃, maintained 10min.
7.4.1.9 Injection volume. 1μL.
7.4.2 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
Liquid cypermethrin, fenvalerate, deltamethrin response value should be within the linear range of the detection instrument. In the chromatographic conditions, standard solutions
FIG blank and high performance liquid chromatography was added the sample solution in Appendix A.
7.5 Blank test
But without addition of the sample, the measurement step is performed in exactly the same operation in parallel.
8 and the result of the calculation expression
Residues in the specimens cypermethrin, fenvalerate, deltamethrin (μg/kg) according to formula (1).
X =
A × cS × V
AS × m
(1)
Where.
--- for the respective X-try feed cypermethrin, fenvalerate, deltamethrin residues, in micrograms per kilogram (μg/kg);
A --- respective sample cypermethrin, fenvalerate, deltamethrin peak area;
CS --- respective standard solution cypermethrin, fenvalerate, deltamethrin concentration, in micrograms per milliliter (μg/mL);
V --- final sample volume in milliliters (mL);
--- the AS standard working solution corresponding peak area cypermethrin, fenvalerate, deltamethrin;
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 1μg/kg.
9.2 Accuracy
This method recoveries on levels 70% to 100% at 1μg/kg ~ 10μg/kg.
9.3 Precision
The relative standard deviation of the method ≤15%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
Description.
1 --- cypermethrin;
2 --- fenvalerate;
3 --- deltamethrin.
Figure A.1 cypermethrin, fenvalerate and deltamethrin chromatogram of the standard solution
(Cypermethrin 50μg/mL, fenvalerate 50μg/mL, deltamethrin 50μg/mL)
Figure A.2 grass carp muscle tissue sample blank chromatogram
Description.
1 --- cypermethrin;
2 --- fenvalerate;
3 --- deltamethrin.
Figure A.3 grass carp muscle tissue blank add cypermethrin, fenvalerate and deltamethrin sample chromatograms
(Cypermethrin 25μg/kg, fenvalerate 25μg/kg, deltamethrin 5025μg/kg)
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