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SN/T 0693-2019 English PDF

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SN/T 0693-2019: (Determination of methoprene residues in foods of plant origin for export)
Status: Valid

SN/T 0693: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
SN/T 0693-2019English329 Add to Cart 3 days [Need to translate] (Determination of methoprene residues in foods of plant origin for export) Valid SN/T 0693-2019
SN 0693-1997English519 Add to Cart 3 days [Need to translate] Method for the determination of methoprene residues in cereals for export Obsolete SN 0693-1997

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Basic data

Standard ID SN/T 0693-2019 (SN/T0693-2019)
Description (Translated English) (Determination of methoprene residues in foods of plant origin for export)
Sector / Industry Commodity Inspection Standard (Recommended)
Classification of Chinese Standard C53
Classification of International Standard 67.050
Word Count Estimation 14,181
Date of Issue 2019
Date of Implementation 2020-07-01
Issuing agency(ies) General Administration of Customs

SN/T 0693-2019: (Determination of methoprene residues in foods of plant origin for export)

---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 methoprene residues in plant food for export The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards Replace SN/T 0693-.1997 Determination of Methoprene Residues in Exported Plant-derived Foods 2019-12-27 release 2020-07-01 Implementation Issued by the General Administration of Customs of the People's Republic of China

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces SN 0693-1997 "method for the inspection of methoprene residues in grains for export". Compared with SN 0693-1997, the main technical changes of this standard are as follows. --The name of the standard was revised from "Methods for the Inspection of Methoprene Residues in Grain Exports" to "Methoprene Residues in Exported Plant-derived Foods" Measurement." --The sampling part has been deleted. --- Added gas chromatography-mass spectrometry as the first method. Compared with SN 0693-1997, this law expands the scope of application of standard testing. It has improved the sample pretreatment technology and lowered the limit of quantification. - SN 0693-1997 as the second method of this standard, that is, liquid chromatography-ultraviolet detector method. --Reduce the limit of quantification, and for different detection objects, the recovery range of multiple levels of methoprene in different matrices is given. Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents. This standard was proposed and managed by the General Administration of Customs of the People's Republic of China. Drafting organization of this standard. China Academy of Inspection and Quarantine. The main drafters of this standard. Wu Yuping, Li Shujuan, Zhang Yang, Li Xiaojuan. The previous editions of the standard replaced by this standard are as follows. Determination of Methoprene Residues in Exported Plant-derived Foods

1 Scope

The first method of this standard specifies the gas chromatography-mass spectrometry method for the determination of methoprene residues in foods of plant origin for export. Second law A liquid chromatographic method for the determination of methoprene residues in grains has been established. The first method of this standard applies to rice, wheat, corn, oranges, grapes, tomatoes, potatoes, spinach, mushrooms, peanuts and tea Determination and confirmation of the residual amount of methoprene in leaves. The second method is suitable for the determination of methoprene residues in brown rice.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version is applicable to this file. For undated reference documents, the latest version (including all amendments) is applicable to this document. GB/T 6682 Analytical laboratory water specifications and experimental methods Method 1 Gas Chromatography-Mass Spectrometry

3 Principle

The sample is extracted by shaking with acetonitrile, and the extract is purified by solid phase extraction, and detected by gas chromatography-mass spectrometry. Time and selective ion qualitative, external standard method for quantification.

4 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade, and the water is the first grade water specified in GB/T 6682. 4.1 Acetonitrile. 4.2 Toluene. chromatographically pure. 4.3 n-hexane. chromatographically pure. 4.4 Acetone. chromatographically pure. 4.5 Sodium chloride. 4.6 Anhydrous sodium sulfate. Burn at 650 ℃ for 4 hours, store in a desiccator, and cool it for later use. 4.7 Acetone-n-hexane solution (37, volume ratio). Measure out 60 mL of acetone and 140 mL of n-hexane, and mix them evenly. 4.8 Acetonitrile-toluene solution (3 to 1, volume ratio). Measure out 60 mL of acetonitrile and 20 mL of toluene, and mix them evenly. 4.9 Methoprene standard material. C19H34O3, CAS number 40596-69-8, purity greater than or equal to 99%. 4.10 Methoprene standard stock solution. accurately weigh 10 mg (accurate to 0.1mg) of methoprene standard substance (4.9) into a 10 mL volumetric flask, Dissolve with acetone (4.4) and dilute to the mark, prepare a standard stock solution with a concentration of 1 mg/mL, and store in a refrigerator at 0 ℃ ~ 4 ℃ in the dark. 4.11 Methoprene standard intermediate solution. accurately draw an appropriate volume of the methoprene standard stock solution (4.10), and prepare a concentrated solution with acetone (4.4). The standard intermediate solution with a concentration of 10.0 mg/L should be stored in a refrigerator at 0 ℃ ~ 4 ℃ and protected from light. 4.12 Methoprene standard working solution. Prepare the standard intermediate solution of methoprene (4.11) with n-hexane to prepare the standard working solution. This working solution needs to be used and prepared. 4.13 Neutral alumina solid phase extraction column. 1 000 mg, 6 mL, or equivalent. 4.14 Graphitized carbon solid phase extraction column. 250 mg, 6 mL, or equivalent. 4.15 TPT solid phase extraction column 1). 2 000 mg, 12 mL, or equivalent. a

5 Equipment

5.1 Gas chromatography-mass spectrometer. equipped with electron impact source (EI). 5.2 Electronic balance. Sensitivity 0.01 mg and 0.01 g. 5.3 Vortex mixer. 5.4 Oscillator. 5.5 Centrifuge. the maximum speed is not less than 5 000 r/min. 5.6 Rotary evaporator. 5.7 Nitrogen blowing concentrator. 5.8 Low-speed centrifuge tube. 50 mL, with lid. 5.9 Sweetheart bottle.

6 Sample preparation and storage

6.1 Sample preparation Grains, nuts and tea samples. Take a representative sample of about 500 g, crush them with a grinder and pass through a 20-mesh sieve; fruits, Vegetable and mushroom samples. Take a representative sample of about 500 g, and homogenize with a homogenizer or tissue masher. After sample preparation, Inside the clean sample bottle, seal and mark it. 6.2 Sample storage Samples of grains, nuts and tea should be stored at 0 ℃~4 ℃, and samples of fruits, vegetables and mushrooms should be kept frozen below -18 ℃. Pumping In the process of sampling and sample preparation, the samples should be prevented from being contaminated or from changing the content of residues.

7 Measurement procedure

7.1 Extraction 7.1.1 Vegetables, fruits and mushrooms. Weigh 5 g sample (accurate to 0.01 g) into a 50 mL centrifuge tube, and add 20 mL acetonitrile (4.1) And 5 g sodium chloride (4.5), shake and extract for 30 min, centrifuge the sample tube at 5,000 r/min for 5 min. Aspirate the supernatant Anhydrous sodium sulfate (4.6) is filtered and collected in a chicken heart bottle, and 20 mL of acetonitrile (4.1) is added to the residue to repeat the above extraction step. Combine the supernatants. Place the extract in a water bath at 40 ℃ by rotary evaporation and concentrate it to near dryness, and then dissolve it with 2 mL of n-hexane (4.3) Residue, to be purified. 7.1.2 Grains and nuts. Weigh 5 g sample (accurate to 0.01 g) into a 50 mL centrifuge tube, add 10 mL of water and soak for 30 min, Add 20 mL acetonitrile (4.1) and 5 g sodium chloride (4.5), shake and extract for 30 min, centrifuge the sample tube at 5 000 r/min 5 min. The supernatant was filtered through anhydrous sodium sulfate (4.6) and collected in a chicken heart bottle. Add 20 mL of acetonitrile (4.1) to the residue. Repeat the above steps and combine the supernatants. Place the extract in a water bath at 40 ℃ by rotary evaporation and concentrate it to near dryness, and then use 2 mL of positive Hexane (4.3) dissolves the residue and is to be purified. 7.1.3 Tea. Weigh 2 g sample (accurate to 0.01 g) into a 50 mL centrifuge tube, add 5 mL of water to soak for 30 min, add 1) TPT solid phase extraction column is the product name of Agela. This information is given for the convenience of users of this standard, and does not mean that Product recognition. If other equivalent products have the same effect, these equivalent products can be used. 20 mL acetonitrile (4.1) and 5 g sodium chloride (4.5) were shaken and extracted for 30 minutes, and the sample tube was centrifuged at 5,000 r/min for 5 minutes. Aspirate the supernatant and filter with anhydrous sodium sulfate (4.6) and collect it in a chicken heart bottle. Add 20 mL of acetonitrile (4.1) to the residue and repeat the process. The above steps, the supernatants were combined. Place the extract in a water bath at 40 ℃ by rotary evaporation and concentrate it to near dryness, and then use 2 mL of n-hexane (4.3) Dissolve the residue and wait to be purified. 7.2 Purification 7.2.1 Vegetables, fruits and grains. connect the graphitized carbon solid phase extraction column (4.14) to the neutral alumina solid phase extraction column (4.13) in series The end is activated with 5 mL acetone-n-hexane solution (4.7) and 5 mL n-hexane (4.3) at a flow rate of 1 mL/min. Will be net Transfer the chemical solution to the serial solid phase extraction column and load the sample, discard the effluent; then wash the chicken heart with 2.5 mL of acetone-n-hexane solution (4.7) Bottle, and transfer the washing liquid to the solid phase extraction column, collect the eluate, repeat the above elution operation three times, pay attention to the Always keep the column from drying out. The eluent was collected and concentrated to near dryness by rotary evaporation in a water bath at 40 ℃, and the volume was dilute with n-hexane (4.3) to 1.0 mL, for GC-MS determination. 7.2.2 Tea. Add anhydrous sodium sulfate (4.6, height about 2 cm) to the TPT solid phase extraction column (4.15), first use 10 mL Acetonitrile-toluene solution (4.8) was activated at a flow rate of 1 mL/min. Transfer the solution to be purified to the solid phase extraction column for loading, and then use 2.5 mL of ethyl acetate The nitrile-toluene solution (4.8) washes the core bottle, and transfers the washing liquid to the solid phase extraction column, and starts to collect the eluate, and repeats The washing and elution operations were performed three times, and finally eluted with 5 mL of acetonitrile-toluene solution (4.8). Collect all eluates in a 40 ℃ water bath strip Concentrate the sample by rotary evaporation to near dryness, and dilute to 1.0 mL with n-hexane (4.3) for GC-MS determination. 7.3 Determination 7.3.1 Gas Chromatography-Mass Spectrometry Conditions 7.3.1.1 Chromatographic column. HP-5 ms, 30.0 m×0.25 mm×0.25 μm, or equivalent performance. 7.3.1.2 Oven heating program. Hold at 50 ℃ for 1 min, and increase the temperature to 280 ℃ at 10 ℃/min for 5 min. 7.3.1.3 Temperature of the injection port. 250 ℃. 7.3.1.4 GC-MS interface temperature. 280 ℃. 7.3.1.5 Carrier gas. helium, purity ≥ 99.999%, constant flow mode. Flow rate. 1.0 mL/min. 7.3.1.6 Sampling mode. no split injection. 7.3.1.7 Injection volume. 2 μL. 7.3.1.8 Ion source temperature. 230 ℃. 7.3.1.9 Quadrupole temperature. 150 ℃. 7.3.1.10 Determination method. Select ion detection method (SIM). 7.3.1.11 Monitoring ion (m/z). 153, 191 (quantitative ion), 278. 7.3.2 Qualitative determination Measure the standard solution and sample solution according to the conditions in 7.3.1.If the retention time of the mass chromatographic peak of the sample solution and the standard solution is not more than Over ±0.5%; in the mass spectrum after subtracting the background, all the selected monitoring ions appear, and the relative abundance of the qualifier ion (using Relative to the intensity percentage of the strongest ion abundance) is consistent with the relative abundance of the standard working solution with the same concentration (m/z 153.m/z 191.m/z 278=100.87.26), the allowable deviation of relative abundance does not exceed the range specified in Table 1, then it can be determined that there are pairs of Should be tested. 7.3.3 Quantitative confirmation Under the best working condition of the instrument in 7.3.1~7.3.2, inject the standard working solution with the chromatographic peak area of the analyte as the ordinate, The concentration of the standard working solution is the abscissa to draw a standard working curve, and use the standard working curve to quantify the chromatographic peaks of the analyte The response value of the chromatographic peak of the analyte in the sample solution should be within the linear range determined by the instrument; if it exceeds the linear range, a proper dilution should be carried out. After release, the sample was injected for determination. Under the above chromatographic conditions, the retention time of methoprene is about 19.0 min, and the selected ion color of the standard product of methoprene For the spectrum, see Figure A.1 in Appendix A. 7.4 Blank test Except that no sample is added, follow steps 7.1 to 7.3.

8 Calculation and expression of results

Gas chromatography-mass spectrometry is used for quantification using standard curve method, and the residual amount of methoprene in the sample is calculated according to formula (1).

9 Limit of quantification and recovery

9.1 Limit of quantification Gas chromatography-mass spectrometry detection method for rice, wheat, corn, orange, grape, tomato, potato, spinach, mushroom and flower The limit of quantification of methoprene in raw materials is 0.01 mg/kg, and the limit of quantification of methoprene in tea is 0.025 mg/kg. 9.2 Addition concentration and recovery rate See appendix B for addition concentration and recovery data. Method 2 Liquid Chromatography-Ultraviolet Detector Method 10 Principle The residual methoprene in the sample was extracted with acetone. After the extract was concentrated, it was dissolved in a n-hexane solution...

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