A kind of recycling method of mycotoxin quechers purification powder
A technology of mycotoxin and purification powder, which is applied in the field of chemical analysis, can solve the problems of QuEChERS purification powder is difficult to handle, the price of QuEChERS purification powder is high, and restricts the development of QuEChERS purification powder, so as to achieve controllable process, low cost and easy operation Effect
Active Publication Date: 2017-09-26
郭礼强
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Problems solved by technology
With the widening and deepening of research on QuEChERS technology, research institutions, scientific research institutions and quality inspection departments of related enterprises have a wide demand for QuEChERS purification powder, coupled with its special production process and stability requirements, resulting in The price of QuEChERS purification powder is still high
Taking the purchase price of Shandong as a reference in 2014, GCB is 4000 yuan / 100g, and ODS is 1300 yuan / 100g. Higher prices restrict the further development of QuEChERS purification powder; QuEChERS purification powder is not easy to handle in nature, and used QuEChERS purification The powder is generally discarded and is a disposable consumable. At present, there is no report on the recycling of QuEChERS purification powder.
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Embodiment 1
[0029] Embodiment 1, a kind of recycling method of mycotoxin QuEChERS purification powder, the use process of QuEChERS purification powder is generally:
[0030] Weigh the crushed sample cornmeal into a centrifuge tube, add acetonitrile water (84:16) and homogenize for 1min, 10000
[0031] Rotation / min Centrifuge for 10min, take 4mL supernatant to a 10mL glass test tube, add 400mg ODS, let it stand for 5min, take 2mL nitrogen to blow dry, use 1mL acetonitrile water (70:30) to make up volume, pass through a 0.22μm filter membrane, and pass through mass spectrometry Detection; the remainder in the glass test tube is a mixture containing ODS purification powder.
[0032] Include the following steps:
[0033] Step 1), collect the used ODS purification powder mixture several times, add 50mL of water, sonicate for 30min, and filter with suction to obtain 23.5g of the purification powder mixture;
[0034] Step 2), fill the purified powder mixture after suction filtration in step 1)...
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The invention discloses a method for recycling mycotoxin QuEChERS purification powder. The used ODS purification powder mixture is collected, added to water, and ultrasonically filtered; the filtered product is filled into a glass tube, and the two ends of the glass tube are sealed and connected to a peek tube. , connect the peek tube reversely and add acetonitrile, discharge the bubbles, and make the liquid level exceed the purification powder; connect the glass tube directly, add acetonitrile solution dropwise from top to bottom; add acetonitrile aqueous solution dropwise from top to bottom, collect the effluent, and recover by vacuum distillation Acetonitrile, add methanol solution dropwise from top to bottom; take out the purification powder mixture from the glass tube, transfer the purification powder to a clean container after centrifugation, add methanol solution again, and ultrasonically filter the obtained purification powder mixture. Using a small amount of acetonitrile and methanol, the recovery cost is relatively low; easy to operate, simple process. The process is controllable and beneficial to the protection of the environment; the recovered purified powder has less impurities and matrix impurities are excluded.
Description
technical field [0001] The invention relates to a mycotoxin QuEChERS purification powder, in particular to a method for recycling the mycotoxin QuEChERS purification powder, which belongs to the field of chemical analysis. Background technique [0002] The QuEChERS word is composed of the initials of the six words Quick, Easy, Cheap, Effective, Rugged and Safe, and was developed by Professor Anastassiades of the United States Department of Agriculture A rapid sample pretreatment technology for agricultural product detection developed by Lehotay et al. in 2003 has been widely concerned in the field of pesticide analysis in food. The key to this method is to adopt the dispersive-SPE purification method. Part of the extract after the organic solvent vibration extraction is directly added to the purification powder for purification. After centrifugation, the supernatant is taken for instrumental analysis. This method replaces the corresponding SPE column purification. The advan...
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IPC IPC(8): G01N1/34
Inventor 郭礼强孙军郝莹宫小明张金玲李凯
Owner 郭礼强