Method for Determination of Metalaxyl and Carbendazim in Wine by Solid-Phase Extraction-LC/MS
A technology of metalaxyl and wine, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of impurity, influence on test results, large matrix interference, etc., and achieve fast extraction speed, high sensitivity, and less impurity interference Effect
Inactive Publication Date: 2017-09-19
中华人民共和国苏州出入境检验检疫局
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[0004] At present, there are no specific national detection standards or related patents for the detection of pesticide residues in wine—metalaxyl, carbendazim, etc. The reports in the literature mainly involve gas chromatography, high performance liquid chromatography, gas chromatography / gas chromatography , liquid chromatography / mass spectrometry, etc., the pretreatment methods mainly use liquid / liquid extraction (Liquid / liquidextraction, LLE), accelerated solvent extraction (Accelerate solvent extraction, ASE), solid phase microextraction (Solid phase microextraction, SPME ) and solid phase extraction (Solidphase extraction, SPE), etc., but wine samples have complex components and large matrix interference. If the pretreatment is not proper, the test results will be easily affected
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[0031] Example: Study on the method for determining the content of carbendazim and metalaxyl in dry red wine by solid phase extraction liquid chromatography-quadrupole tandem mass spectrometry.
[0032] 1 Materials and methods
[0033] 1.1 Instruments and reagents:
[0034] API TripleQuad 4500 ultra-high performance liquid chromatography-tandem quadrupole mass spectrometer (AB SCIEX company), XS105 balance (Mettler Toledo), NH2 solid phase extraction column (1g / 6ml, American waters company).
[0035] Carbendazim (carbendazim, CAS No.10605-21-7, standard), metalaxyl (Metalaxyl, CASNo.57837-19-1, standard), acetonitrile (Acetonitrile, HPLC grade), sodium chloride (Sodium chloride, GR grade), toluene (Methylbenzene, HPLC grade), distilled water made by the laboratory.
[0036] 1.2 Instrument conditions
[0037] The measurement conditions of ultra-high performance liquid chromatography-tandem quadrupole mass spectrometer are: chromatographic column: Inertsil C8, 5 μm, 150mm*2.1...
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The invention discloses a method for measuring metalaxyl and carbendazim in wine by solid-phase extraction liquid-mass spectrometry. After the solution is salted out, extract the acetonitrile layer with a solid-phase extraction column, elute through the solid-phase extraction column, collect the purified eluent, and then transfer it to a rotary evaporator for concentration, dry the concentrated solution with nitrogen, and dissolve it back through the acetonitrile aqueous solution Finally, inject liquid mass spectrometer to analyze, promptly obtain the step of the content of metalaxyl and carbendazim in wine. This method has the outstanding advantages of less organic solvent consumption, fast extraction speed, less impurity interference, and high sample recovery rate, and can provide technical support for the establishment of effective pesticide safety limit control and risk management for wine.
Description
technical field [0001] The invention relates to the technical field of product safety and detection, in particular to a method for detecting pesticide residues in wine by solid phase extraction liquid mass spectrometry. Background technique [0002] Wine is made from fresh grapes or grape juice after fermentation. Wine is rich in various nutrients, such as amino acids, vitamins, β-sitosterol, polyphenols and mineral elements. Appropriate drinking of wine can prevent diseases and enhance human health. However, in the process of controlling grape diseases and insect pests, pesticides such as insecticides, fungicides and herbicides are often sprayed. Generally speaking, pesticides have a relatively long residual period and are accompanied by certain toxicity. Such residual pesticides will eventually enter the human body through the food chain, bringing potential harm to human health. [0003] With the improvement of detection technology and food quality and safety requirements...
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IPC IPC(8): G01N30/02G01N30/08
Inventor 陈军樊继鹏谢鑫陟徐罕琦
Owner 中华人民共和国苏州出入境检验检疫局