Method for the determination of captan residues in fruits for export

This standard specifies the sampling, sample preparation and high performance liquid chromatography method for the inspection of captan residues in exported fruits. This standard applies to the inspection of captan residues in exported apples. SN 0654-1997 Inspection method for captan residues in exported fruits SN0654-1997 Standard download decompression password: www.bzxz.net
This standard specifies the sampling, sample preparation and high performance liquid chromatography method for the inspection of captan residues in exported fruits. This standard applies to the inspection of captan residues in exported apples.

This standard is the first of its kind in China. 1 Scope 1 Method for the preparation and presentation of captan residues in fruits for export SH 0654—1997 The first part of the standard is the basic rules for the preparation of captan residues in fruits for export. It is formulated to improve the sensitivity of the standard formulation method and the amount of captan residues and the biological activity of the standard. The attached industry standard for the reminder was proposed by the National Import and Export Commodity Inspection Bureau and coordinated by "Zhiming, Zheng Ruxi, Gao Zhiwei.
, sample preparation and high performance liquid chromatography determination method. The test of the residue of captan in apples in exported fruits!
This standard applies to export
2 Sampling and sampling
2.1 Inspection batches
kidney oranges should be easy to identify the same characteristics, such as packaging, marking, origin, specifications and other aspects. 2.2 Sampling quantity
Minimum sampling quantity 2.5. Cut the new film into 11 parts, crush them with a tissue crusher, divide them into two parts, and put them into a clean container as the sample. Seal and mark them. During the following diagnostic process, the sample must be sent to the laboratory to prevent contamination or changes in the residue content. 3. Determination method: The acetone is used to extract the glandular glands, extract the cancer, and then the extract is connected with β*1-E C. Purify. Wash the muscle with enzyme acetylcholine, adjust the volume, and reduce the eluate. Then use a high performance liquid chromatograph with an external detector to measure. The reagents used for external standard method are all analytically pure, and the water is distilled water. Energy
liquid: weigh 0.1g0 accurately to 0.000
00 2g) of captan standard in a 100mL volumetric flask, dissolve it with an appropriate amount of methanol, dilute it to the mark with methanol, and mix well. Prepare the appropriate amount of captan standard stock solution accurately and dilute it with methanol to a standard working solution of appropriate concentration. The standard working solution needs to be prepared once a week. There is a UV detector
Island broken batch
Wash it with 2mL of water
Determination step
The concentrated extract is poured
and then transferred to 2mT
with methanol
Filling phase: methanol-2
Phase chromatography
Except for unweighed
Add 50mL of acetone and shake it on an oscillator for 1h. The extract is filtered with a Buchner funnel and divided into three parts with about 40mL of acetone
Use a box mass spectrometer
|tt||g purification column, wash away water-soluble impurities with 10mL water. Elute with 10mL methanol, collect the eluate in a 10mL centrifuge tube, blow it to a nearly dry bottle with nitrogen, and settle. Filter with a filter membrane, and the filtrate is used for high-performance liquid chromatography-mass spectrometry. m inner diameter
When the captan is retained
, all are carried out according to the above determination steps
Use a chromatographic data processor or calculate the residual content of captan in the sample according to formula (1):.
In the formula:
The peak height of captan in the sample full of Glaube
s-standard working solution, m sample solution final
The sample solution
Note: Calculation results
4 Determination limit and recovery rate of the method
4.1 Determination
Since the determination limit is 0.3mgkg.
The experimental data of the recovery rate of captan in apple
inch, the recovery rate is 84.6:
At 3.0mgkg, the recovery rate is 96. 1 The content and the test sample
Appendix A
(Suggested Appendix)
Standard product chromatogramwwW.bzxz.Net
Figure A1 Liquid chromatogram of captan standard product
Appendix
Linear range of the instrument detection
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