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A technology of solid-phase extraction column and mixed matrix, which is applied in the direction of solid adsorbent-liquid separation, material separation, instruments, etc., and can solve problems such as different mechanisms of action
Inactive Publication Date: 2011-05-11
INST OF MEDICINAL PLANT DEV CHINESE ACADEMY OF MEDICAL SCI
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At present, there are many kinds of packing matrices for solid-phase extraction columns, and thei
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Embodiment 1
[0014] Embodiment one: the specific steps of a preferred embodiment of the present invention are:
[0015] (1) Selection of solid phase extraction column empty tube and sieve plate
[0016] Choose standardized 15ml empty tubes and polyethylene sieve plates. The bottom sieve plate is thin, and the upper sieve plate of the filler is thicker.
[0017] (2) The proportion of filler and the selection of filling amount
[0018] The ratio of pvpp and Florisil loading is 2 to 1, and the total filling amount of the matrix is 1.5g.
[0019] (3) Filling of solid phase extraction column
[0020] The filling of the column includes the following steps: a. Put a polyethylene sieve plate in the bottom of the solid phase extraction column empty tube, b. Fill in a certain amount of pvpp and Florisil mixed matrix, dry the column, c. Put a polyethylene sieve plate, d. Press the packing properly, the sieve plate should not be skewed, and the SPE column is completed.
[0021] (4) Selection of ...
Embodiment 2
[0024] Embodiment two: the content of patulin in apple products and hawthorn juice is determined by patulin solid phase extraction column high performance liquid chromatography:
[0025] (1) Prepare a patulin solid-phase extraction column by the same method as in Example 1.
[0026] (2) In the blank samples (apple juice, applesauce, hawthorn juice) that do not contain patulin, add patulin standard substance at three levels of 25ug / kg, 50ug / kg, and 250ug / kg respectively.
[0027] (3) Sample processing
[0028] Applesauce: Take 5g of applesauce sample, add 5ml of water, add pectinase solution (activity not less than 1500IU / g) and place it at 40°C for 2 hours, or at room temperature for 16 hours. After adding 20ml of acetonitrile, vibrate on a vortex shaker for 2 minutes, take the supernatant directly through the solid phase extraction column, and collect 5ml of the filtrate. Blow dry with nitrogen at 40°C, add 200ul mobile phase to dissolve, pass through a microporous membrane...
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Abstract
The invention discloses a solid phase extraction and purification column, which is used in pretreatment during detection of patulin, is mainly applied to the detection of patulin residues and belongs to the field of solid phase extraction columns. An appropriate amount of crosslinked polyvinylpyrrolidone (pvpp) is uniformly mixed with Florisil, and the mixture is filled into a solid phase extraction column hollow pipe with the volume of 15ml. Product extracting solution of hawthorn and apples directly passes through the solid phase extraction column, filtrate is collected and dried by nitrogen, volume is fixed and filtering is performed for analyzing. The column has good impurity removing effect and high yield and can effectively replace the effect of a 228AflaPat multifunctional column on the detection of the patulin. The effect of the solid phase extraction column is basically equivalent to that of the 228AflaPat multifunctional column, and the cost of the solid phase extraction column is one tenth of that of the 228AflaPat multifunctional column. The column is easy and convenient to prepare, is easy to operate, has high repeatability and is easy for mass production.
Description
Technical field: [0001] The invention relates to a preparation method of a solid phase extraction column, in particular to a solid phase extraction column (SPE) for purifying patulin and filled with pvpp and Florisil mixed matrix. Background technique: [0002] Patulin is a toxic fungal metabolite that is widely distributed in nature and mainly contaminates fruits and their products, especially apples, hawthorns, pears, tomatoes, apple juice, hawthorn slices, etc. Toxicological tests have shown that patulin has toxic effects such as fertility, carcinogenesis and immunity, and it is also a neurotoxin. In most European and American countries, the limit standard of patulin is 0-50 μg / kg; WHO recommends that the maximum limit standard of patulin in apple juice is 50 μg / kg; the corresponding standard in my country stipulates that the limit standard of apple and hawthorn semi-finished products is 100 μg / kg, the limit standard for fruit juice, jam, fruit wine, canned food and pres...
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IPC IPC(8): B01D15/08B01D15/22G01N30/06C07D493/04
Inventor 杨美华周玉春
Owner INST OF MEDICINAL PLANT DEV CHINESE ACADEMY OF MEDICAL SCI
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