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Solid-phase extraction column and solid-phase extraction column filling material production method and method for detecting aflatoxin by using solid-phase extraction column thereof

A solid-phase extraction column and aflatoxin technology, which is applied in the production of solid-phase extraction column and solid-phase extraction column packing, and in the field of detection of aflatoxin, can solve problems such as false positives, high detection costs, and cumbersome processing operations, and achieve Good reproducibility and stability, low detection cost, and short processing time

Active Publication Date: 2018-08-24
甘肃省商业科技研究所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TLC operation is complicated, the concentration of AFM1 standard product is high, the potential contamination is high, the specificity is poor, the sensitivity is also relatively poor, the detection time is long, the detection limit is 0.3 μg, and the sample recovery rate is 67% (fresh milk) , and 80% (milk powder), not suitable for mass sample testing
Analytical methods requiring extraction and purification Sample pretreatment operations are cumbersome, complex, time-consuming, and labor-intensive
High performance liquid chromatography (HPLC) has a high degree of automation, good stability, and high sensitivity, but requires a large investment in equipment, high operational technical requirements, high purification column consumption, high detection costs, and low specificity of immunoaffinity columns. Good, but quantitative detection needs to be combined with HPLC instrument and fluorescence photometer, and the detection technical requirements and cost are relatively high. Compared with ELISA method, the operation is simple, fast, less polluted, and the sensitivity is also high. It is suitable for general inspection of batch samples and screening, but there may be false positives and false negatives, and only semi-quantitative

Method used

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  • Solid-phase extraction column and solid-phase extraction column filling material production method and method for detecting aflatoxin by using solid-phase extraction column thereof
  • Solid-phase extraction column and solid-phase extraction column filling material production method and method for detecting aflatoxin by using solid-phase extraction column thereof
  • Solid-phase extraction column and solid-phase extraction column filling material production method and method for detecting aflatoxin by using solid-phase extraction column thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method of solid phase extraction packing:

[0031] 1. Carrier synthesis: Add 75g of distilled water and 1g of polyvinyl alcohol powder into a 250ml three-neck flask, stir and dissolve them well as the dispersed phase for later use. Precisely measure 15g of toluene, 5g of n-octane, 9g of N-vinylpyrrolidone and 15g of divinylbenzene into a small beaker, add 0.15g of azobisisobutyronitrile and mix well, then pour into a three-necked flask, stir rapidly for 30min, and heat to 70 ℃ condensed and refluxed, stirred and reacted at 1000r / min for 12h, then stopped the reaction, washed the product with water and methanol, and dried it in vacuum at 80°C for 4h to obtain divinylbenzene-N-vinylpyrrolidone copolymer microspheres. The spherical particle size is 30-50μm.

[0032] 2. Synthesis of ionic liquid: Weigh 25g of N-methylimidazole and 26g of 1-chloro-n-octane in a 100mL flask, heat to reflux for 10h, wash the reacted liquid with hot ethyl acetate several times,...

Embodiment 2

[0039] The preparation method of solid phase extraction packing:

[0040] 1. Carrier synthesis: Add 70 g of distilled water and 1 g of polyvinyl alcohol powder into a 250 ml three-neck flask and stir to dissolve them as a dispersed phase for later use. Precisely measure 15g of toluene, 5g of n-octane, 9g of N-vinylpyrrolidone and 15g of divinylbenzene into a small beaker, add 0.15g of azobisisobutyronitrile and mix well, then pour into a three-necked flask, stir rapidly for 25min, and heat to 65 ℃ reflux, stirring and reacting at 1000r / min for 11.5h, then stop the reaction, wash the product with water and methanol, and dry it in vacuum at 75°C for 3.5h to obtain divinylbenzene-N-vinylpyrrolidone copolymer microspheres. The particle size of the microspheres is 30-50 μm.

[0041] 2. Synthesis of ionic liquid: Weigh 25g of N-methylimidazole and 26g of 1-chloro-n-octane in a 100mL flask, heat to reflux for 10h, wash the reacted liquid with hot ethyl acetate several times, discard...

Embodiment 3

[0049] The preparation method of solid phase extraction packing:

[0050] 1. Carrier synthesis: Add 80 g of distilled water and 1 g of polyvinyl alcohol powder into a 250 ml three-necked flask and stir to dissolve them as a dispersed phase for later use. Precisely measure 15g of toluene, 5g of n-octane, 9g of N-vinylpyrrolidone and 15g of divinylbenzene into a small beaker, add 0.15g of azobisisobutyronitrile and mix well, then pour into a three-necked flask, stir rapidly for 35min, and heat to 75 ℃ condensed and refluxed, stirred and reacted at 1000r / min for 12.5h, then stopped the reaction, washed the product with water and methanol, and dried in vacuum at 85°C for 4.5h to obtain divinylbenzene-N-vinylpyrrolidone copolymer microspheres. The particle size of the microspheres is 30-50 μm.

[0051] 2. Synthesis of ionic liquid: Weigh 25g of N-methylimidazole and 26g of 1-chloro-n-octane in a 100mL flask, heat to reflux for 10h, wash the reacted liquid with hot ethyl acetate se...

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Abstract

The invention discloses a solid-phase extraction column and a solid-phase extraction column filling material production method and a method for detecting aflatoxin by using the solid-phase extractioncolumn thereof, which belong to the field of food detection. The solid-phase extraction column comprises a solid-phase extraction column sleeve, an injection sample-introduction port, and a liquid outlet, a cover is arranged at the solid-phase extraction column sleeve, the injection sample-introduction port is arranged at the cover, an upper glass fiber baffle plate and a lower glass fiber baffleplate are arranged in an inner chamber of the solid-phase extraction column sleeve, and a solid-phase extraction mixed filling material is placed between the upper glass fiber baffle plate and the lower glass fiber baffle plate. The method for producing the solid-phase extraction column filling material comprises a carrier synthesis step and an ionic liquid immobilization step. The processing timeof the superfast solid-phase extraction column is short, the detection cost is low, and the method has good reappearance and stability. The rapid extraction method completely uses a high-efficiency extraction technology, which is stable and fast. The solid-phase extraction column is used for detecting the content of aflatoxin in milk and a dairy product.

Description

technical field [0001] The invention belongs to the field of food testing, and in particular relates to a manufacturing method of a solid-phase extraction column and a filler of the solid-phase extraction column and a method for detecting aflatoxin by using the solid-phase extraction column. Background technique [0002] Aflatoxin M1 (AFM1) belongs to a class of structurally similar compounds called Aflatoxins, which are metabolites produced by the common fungi Asperillus Flavus and Asperillus Parasiticus Among them, aflatoxin B1 (AFB1) is the most important toxin. After mammals ingest feed or food contaminated by AFB1, AFM1 is generated under the catalysis of the liver microsomal monooxygenase system in the body. AFM1 is also directly produced by some Aspergillus flavus and Aspergillus parasitica. The toxicity of AFM1 is mainly manifested in carcinogenicity and mutagenicity. Studies on the physiological carcinogenic mechanism have shown that the epoxy structure of the fura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01D15/20B01J20/286G01N30/02G01N30/06
CPCB01D15/206B01D15/22B01J20/286G01N30/02G01N30/06G01N2030/062
Inventor 邓丽娟
Owner 甘肃省商业科技研究所有限公司
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