Preparation method of bensulfuron methyl molecularly imprinted polymer and application thereof

Abstract

The invention relates to a preparation method of bensulfuron methyl molecularly imprinted polymer and application thereof. The preparation method includes steps of dissolving one or more functional monomers and bensulfuron methyl in a solvent, respectively adding a crosslinking agent, an initiator and a dispersing agent, mixing and dissolving by supersonic wave, aerating N2 to protect, heating orusing ultraviolet radiation to initiate polymerization reaction, eluting template molecule, and drying in vacuum to obtain the bensulfuron methyl molecularly imprinted polymer. The purification and enrichment effects of the bensulfuron methyl molecularly imprinted polymer to sulfonylurea herbicides is obviously better than present nonspecific C18 column, silica gel column, and magnesium silicate column, thereby increasing detection limit and sensitivity of analysis instrument.

Description

Technical field

[0001] The invention relates to the technical field of polymer synthesis. More specifically, the present invention belongs to analysis and detection technology, and relates to the preparation method and application of bensulfuron-methyl molecularly imprinted polymer.

Background technique

[0002] Sulfonylurea herbicides have been commercially produced in the 1980s since the first variety, Chlorsulfuron-methyl, was developed by Dr. Levitt of DuPont Company in the United States in 1978. Due to its high efficiency, broad-spectrum, and low Toxicity and other advantages, and then after the structure of chlorsulfuron was modified, more than 30 varieties have been invented. There are 21 varieties of sulfonylurea herbicides commonly used in my country, which have become rice, corn, soybean, rapeseed, wheat And the leading varieties of weed control in lawn, woodland, non-cultivated land and some dry land crops. It has a good control effect on rice and dryland gras...

Examples

Embodiment 1

[0078] Preparation of Bensulfuron-methyl Molecularly Imprinted Polymer

[0079] The preparation method is described as follows:

[0080] (1) Polymerization steps:

[0081] 0.4071 g of bensulfuron-methyl and 500 μL of methacrylic acid were dissolved in 50 mL of dichloromethane, and the mixture was degassed by ultrasonic wave for 3 min. Mix overnight at a temperature of 10°C;

[0082] Then above-mentioned mixture is transferred in the three-necked bottle, add 1.1704g trimethylolpropane trimethacrylate crosslinking agent, 0.2090g 2,2-dimethoxy-2-phenylacetophenone photoinitiator respectively and 0.1127g dichloromethane, then ultrasonically mix to dissolve completely, fill with N 2 Protection, at a stirring speed of 60r / min and at room temperature, the polymerization reaction was carried out under the initiation of ultraviolet light for 24h. After the polymerization reaction, it was repeatedly washed with acetone several times to remove fine particles and unreacted substances,...

Embodiment 2

[0093] (1) Preparation of MISPE column:

[0094] Weigh 200 mg of the bensulfuron-methyl molecularly imprinted polymer prepared in Example 1, fill it into a 3ml solid-phase extraction empty column, and place 0.45 μm sieve plates at the upper and lower ends of the column to obtain the bensulfuron-methyl molecularly imprinted solid-phase extraction column MISPE; MISPE column should be activated with 5ml of dichloromethane before use;

[0095] (2) MISPE-HPLC determination of Taihu Lake rice samples:

[0096] In order to compare MISPE column with ENVI TM The purification effect of 18-SPE column, using MISPE column and ENVI TM The 18-SPE column was used to determine the recovery rate of the enrichment and purification effect of rice samples added with standard substances BSM, MSM, NS and TBM. BSM, MSM, NS and TBM are all prepared as a mixed standard acetonitrile solution of about 2.5 μg / mL.

[0097] Rice sample extraction pretreatment: Weigh about 5g of rice sample that has been...

Embodiment 3

[0106] The embodiment of this example is the same as Example 2, except that the MISPE-HPLC determination of soybean samples is carried out.

[0107] Soybean samples were spiked with BSM, MSM, NS and TBM at concentrations of 20ng / g and 40ng / g, MISPE column and ENVI TM The 18-SPE column eluate was concentrated 10 times before HPLC analysis, using MISPE and ENVI TM The high performance liquid chromatogram of the soybean sample pretreated by the 18-SPE column is shown in the appendix Figure 4 . Table 5 shows the spiked soybean samples using MISPE and ENVI respectively TM The recovery rate after 18-SPE column pretreatment, as can be seen from Table 5 results, adopts the BSM recovery rate of MISPE column pretreatment to be the highest, and the recovery rate of 20ng / g and 40ng / g to the standard addition concentration all reaches 100%, higher than ENVI TM The recovery rate of 18-SPE column, but the recovery rate of TBM pretreated by MISPE column is lower than that of ENVI TM 18-...

Technical field

[0001] The invention relates to the technical field of polymer synthesis. More specifically, the present invention belongs to analysis and detection technology, and relates to the preparation method and application of bensulfuron-methyl molecularly imprinted polymer.

Background technique

[0002] Sulfonylurea herbicides have been commercially produced in the 1980s since the first variety, Chlorsulfuron-methyl, was developed by Dr. Levitt of DuPont Company in the United States in 1978. Due to its high efficiency, broad-spectrum, and low Toxicity and other advantages, and then after the structure of chlorsulfuron was modified, more than 30 varieties have been invented. There are 21 varieties of sulfonylurea herbicides commonly used in my country, which have become rice, corn, soybean, rapeseed, wheat And the leading varieties of weed control in lawn, woodland, non-cultivated land and some dry land crops. It has a good control effect on rice and dryland gras...

Examples

Embodiment 1

[0078] Preparation of Bensulfuron-methyl Molecularly Imprinted Polymer

[0079] The preparation method is described as follows:

[0080] (1) Polymerization steps:

[0081] 0.4071 g of bensulfuron-methyl and 500 μL of methacrylic acid were dissolved in 50 mL of dichloromethane, and the mixture was degassed by ultrasonic wave for 3 min. Mix overnight at a temperature of 10°C;

[0082] Then above-mentioned mixture is transferred in the three-necked bottle, add 1.1704g trimethylolpropane trimethacrylate crosslinking agent, 0.2090g 2,2-dimethoxy-2-phenylacetophenone photoinitiator respectively and 0.1127g dichloromethane, then ultrasonically mix to dissolve completely, fill with N 2 Protection, at a stirring speed of 60r / min and at room temperature, the polymerization reaction was carried out under the initiation of ultraviolet light for 24h. After the polymerization reaction, it was repeatedly washed with acetone several times to remove fine particles and unreacted substances,...

Embodiment 2

[0093] (1) Preparation of MISPE column:

[0094] Weigh 200 mg of the bensulfuron-methyl molecularly imprinted polymer prepared in Example 1, fill it into a 3ml solid-phase extraction empty column, and place 0.45 μm sieve plates at the upper and lower ends of the column to obtain the bensulfuron-methyl molecularly imprinted solid-phase extraction column MISPE; MISPE column should be activated with 5ml of dichloromethane before use;

[0095] (2) MISPE-HPLC determination of Taihu Lake rice samples:

[0096] In order to compare MISPE column with ENVI TM The purification effect of 18-SPE column, using MISPE column and ENVI TM The 18-SPE column was used to determine the recovery rate of the enrichment and purification effect of rice samples added with standard substances BSM, MSM, NS and TBM. BSM, MSM, NS and TBM are all prepared as a mixed standard acetonitrile solution of about 2.5 μg / mL.

[0097] Rice sample extraction pretreatment: Weigh about 5g of rice sample that has been...

Embodiment 3

[0106] The embodiment of this example is the same as Example 2, except that the MISPE-HPLC determination of soybean samples is carried out.

[0107] Soybean samples were spiked with BSM, MSM, NS and TBM at concentrations of 20ng / g and 40ng / g, MISPE column and ENVI TM The 18-SPE column eluate was concentrated 10 times before HPLC analysis, using MISPE and ENVI TM The high performance liquid chromatogram of the soybean sample pretreated by the 18-SPE column is shown in the appendix Figure 4 . Table 5 shows the spiked soybean samples using MISPE and ENVI respectively TM The recovery rate after 18-SPE column pretreatment, as can be seen from Table 5 results, adopts the BSM recovery rate of MISPE column pretreatment to be the highest, and the recovery rate of 20ng / g and 40ng / g to the standard addition concentration all reaches 100%, higher than ENVI TM The recovery rate of 18-SPE column, but the recovery rate of TBM pretreated by MISPE column is lower than that of ENVI TM 18-...

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