Extraction and purification method for determining organophosphorus pesticide residues in fruits and vegetables
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A technology for organophosphorus pesticides, vegetables and fruits, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of increasing method application steps, increasing environmental pollution, and increasing detection labor, so as to reduce dosage, improve detection efficiency, reduce Detection steps and human effect
Inactive Publication Date: 2013-09-18
浙江省林产品质量检测站
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The application of various solid-phase extraction purification cartridges will inevitably increase the amount of organic reagents, increase environmental pollution, and at the same time increase the application steps of the method and increase the workload of detection
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Embodiment 1
[0029] An extraction and purification method for the determination of organophosphorus pesticide residues in fruits and vegetables, taking bayberry as an example, such as figure 1 As shown, it consists of the following steps in turn:
[0030] A. Accurately weigh 25g of ground fruit and vegetable samples in a 100ml centrifuge tube;
[0031] B. Accurately add 50ml of acetonitrile extract;
[0032] C. Use a homogenizer to disperse and extract at a speed of 10kr / min for 1min, then add 5g of sodium chloride, cover and shake vigorously for 10s;
[0033] D. Stand still for 30 minutes, and purify after the stratification is clear;
[0034] E. Take 10ml of supernatant and purify it through MycoSep 226 AflaZon+ column;
[0035] F. Take 1ml of the purified acetonitrile extract in the sample bottle, and wait for the determination on the machine.
[0036] The acetonitrile extract purified by MycoSep 226 AflaZon+ purification cartridge is colorless and transparent, which can significant...
Embodiment 2
[0038] An extraction and purification method for the determination of organophosphorus pesticide residues in fruits and vegetables, adding dichlorvos, profenofos, acephate, acephate, phorate, and oxymethol with a mass concentration of 0.08mg / kg to bayberry, cucumber, and pepper Fruit, diazinon, monocrotophos, dimethoate, dimethophos, parathion, fenthion, isofenfos, isocarbophos, quinalphos, methion, ethion, 19 kinds of organophosphorus pesticides such as thionon, the spiked recovery spectra obtained under the following chromatographic conditions, the results are as follows: Figures 2 to 4 shown. In the prior art, the chromatogram of the 10th injection of the cucumber sample that was not purified by the MycoSep 226 AflaZon+ purification column was spiked and recovered, and the type and concentration of the added pesticides were consistent with those of the present invention. Such as Figure 5 shown. And comparing the result spectrogram of the present invention with the prio...
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Abstract
The invention belongs to the technical field of pesticide residue determination, relates to a vegetable and fruit pesticide residue pre-treatment method and in particular relates to an extraction and purification method for determining organophosphorus pesticide residues in fruits and vegetables. The extraction and purification method comprises the following steps of: sampling, adding an acetonitrile extracting solution, purifying by virtue of a MycoSep 226 AflaZon+ small column, and then determining. According to the extraction and purification method, dosage of an organic reagent is reduced, and nitrogen blowing or rotary steaming equipment is not required; a step of detecting organic phosphorus in a conventional method is not required, manpower is reduced, and detection efficiency is improved; purification degree of an organic phosphorus extracting solution is obviously improved, the obtained sample injection solution is clear and transparent, no obvious pollution on a detection system is produced after sample injection is carried out for multiple times, sensitivities of instrument and equipment are consistent, and a detection limit is constant; and peak height is not reduced and peak shape is constant after the sample injection is carried out for multiple times even if residues of organophosphorus pesticides, such as methamidophos, acephate, moncrotophos and omethoate with strong polarity, are determined. The extraction and purification method for detecting organophosphorus pesticide residues in fruits and vegetables has a good application prospect in the technical field of pesticide residue determination.
Description
technical field [0001] The invention belongs to the technical field of determination of pesticide residues, relates to a method for pretreatment of pesticide residues in vegetables and fruits, in particular to an extraction and purification method for determination of organophosphorus pesticide residues in fruits and vegetables. Background technique [0002] Fruits and vegetables are important food sources in people's daily life. With the improvement of people's quality of life, people's awareness of food safety has been continuously enhanced, especially in recent years. sensitive. Pesticide residues in fruits and vegetables are a common problem. When organochlorine pesticides have been discontinued, organophosphorus pesticides have become the main source of pesticide pollution in vegetables. Even supermarkets cannot guarantee safety. A large number of pesticides left on vegetables not only directly poison the human body, but also cause acute poisoning or lead to the accumu...
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