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Preparation method of dumbbell-shaped molecular imprinting stirring rod

A molecular imprinting and stirring rod technology, applied in the field of analysis and detection, can solve problems such as interference and lack of selectivity, and achieve the effects of increasing binding sites, speeding up analysis, and reducing thickness

Inactive Publication Date: 2013-05-22
NANJING MEDICAL UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Traditional PDMS coatings are only suitable for non-polar and low-polarity analytes, lack of selectivity, and will suffer serious interference in complex sample matrices

Method used

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  • Preparation method of dumbbell-shaped molecular imprinting stirring rod
  • Preparation method of dumbbell-shaped molecular imprinting stirring rod
  • Preparation method of dumbbell-shaped molecular imprinting stirring rod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 哑铃状搅拌棒(棒体直径1.4mm,球体直径2mm,长度1.2cm)在0.5mol / L氢氧化钠中浸泡1h、0.1mol / L盐酸中浸泡1h,去离子水清洗除去表面残留的酸至中性,60℃真空干燥活化2h,干燥后放于质量百分比浓度为20%的γ-氨丙基三乙氧基硅烷乙醇溶液中硅烷化1.5h,乙醇洗净,再置入质量百分比浓度为50%的三羟甲基丙烷三丙烯酸酯甲醇溶液反应4h,甲醇洗净,60℃真空干燥备用。

[0039] 0.3mmol伐地那非和103.0uL甲基丙烯酸在30mL甲苯甲醇(v:v / 4:1)中溶液中混匀后,预聚12h,加入30mg偶氮二异丁腈以及7.2mmol EGDMA(使得替代模板分子、功能单体、交联剂三者的摩尔比为1:4:24。取2mL上述混合溶液于玻璃瓶中,将哑铃状搅拌棒浸入溶液中,通氮气除氧,塞紧密封,氮气环境下55℃聚合6h。上述聚合反应重复进行4次。取出哑铃状搅拌棒,真空60℃老化1h,甲醇乙酸溶液(9:1,v:v)洗脱模板分子,直至高效液相色谱紫外检测器检测不到模板分子为止。

Embodiment 2

[0041] 哑铃状搅拌棒(棒体直径1.4mm,球体直径2mm,长度1.2cm)在1mol / L氢氧化钠中浸泡1h、0.5mol / L盐酸中浸泡1h,去离子水清洗除去表面残留的酸至中性,60℃真空干燥活化2h,干燥后放于质量百分比浓度为25%的γ-氨丙基三乙氧基硅烷乙醇溶液中硅烷化1.5h,乙醇洗净,再置入质量百分比浓度为50%的三羟甲基丙烷三丙烯酸酯甲醇溶液反应4h,甲醇洗净,60℃真空干燥备用。

[0042] 0.3mmol伐地那非和103.0uL甲基丙烯酸在30mL甲苯甲醇(v:v / 4:1)中溶液中混匀后,预聚12h,加入30mg偶氮二异丁腈以及7.2mmol EGDMA(使得替代模板分子、功能单体、交联剂三者的摩尔比为1:4:24。取2mL上述混合溶液于玻璃瓶中,将哑铃状搅拌棒浸入溶液中,通氮气除氧,塞紧密封,氮气环境下55℃聚合6h。上述聚合反应重复进行4次。取出哑铃状搅拌棒,真空60℃老化2h,甲醇乙酸溶液(9:1,v:v)洗脱模板分子,直至高效液相色谱紫外检测器检测不到模板分子为止。

Embodiment 3

[0044] 哑铃状搅拌棒(棒体直径1.4mm,球体直径2mm,长度1.2cm)在1mol / L氢氧化钠中浸泡1h、0.1mol / L盐酸中浸泡1h,去离子水清洗除去表面残留的酸至中性,60℃真空干燥活化2h,干燥后放于质量百分比浓度为30%的γ-氨丙基三乙氧基硅烷乙醇溶液中硅烷化1.5h,乙醇洗净,再置入质量百分比浓度为70%的三羟甲基丙烷三丙烯酸酯甲醇溶液反应4h,甲醇洗净,60℃真空干燥备用。

[0045] 0.3mmol伐地那非和103.0uL甲基丙烯酸在30mL甲苯甲醇(v:v / 4:1)中溶液中混匀后,预聚12h,加入30mg偶氮二异丁腈以及7.2mmol EGDMA(使得替代模板分子、功能单体、交联剂三者的摩尔比为1:4:24。取2mL上述混合溶液于玻璃瓶中,将哑铃状搅拌棒浸入溶液中,通氮气除氧,塞紧密封,氮气环境下55℃聚合6h。上述聚合反应重复进行4次。取出哑铃状搅拌棒,真空60℃老化4h,甲醇乙酸溶液(9:1,v:v)洗脱模板分子,直至高效液相色谱紫外检测器检测不到模板分子为止。

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Abstract

The invention discloses a preparation method of a dumbbell-shaped molecular imprinting stirring rod. The method comprises the following steps of: dipping on the dumbbell-shaped stirring rod in alkali and acid in turn for carrying out activation and silanization reaction; further dipping the dumbbell-shaped stirring rod into a trimethylolpropane tricrylic acid ester solution to carry out grafting reaction; putting a template molecule vardenafil and a functional monomer into a pore-foaming agent for prepolymerization, subsequently adding a cross-linking agent and an initiator and putting into the grafted dumbbell-shaped stirring rod to polymerize; repeating the polymerization reaction of the dumbbell-shaped stirring rod, further aging, and finally washing the template molecules so as to obtain the dumbbell-shaped molecular imprinting stirring rod. The stirring rod prepared by using the preparation method is combined with a chromatograph and can be applied to rapid separation and enrichment of nafil compounds in complex matrixes such as food, medicines and health-care products, so that accurate detection on a sample, with high selectivity and high sensitivity, is achieved.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a preparation method of a dumbbell-shaped molecularly imprinted stirring rod using vardenafil as a template molecule. Background technique [0002] With the improvement of living standards, people's requirements for health are getting higher and higher, so the safety of health care products has received extensive attention. The purpose of purchasing health products is to strengthen the body and supplement the various nutrients that the human body lacks. However, in order to highlight the efficacy and attract consumers, many health products randomly add chemicals that have quick results in a short period of time but have serious side effects. Especially health food. In order to achieve immediate results, kidney and yang health care products often add some chemicals for the treatment of male sexual dysfunction, such as sildenafil citrate, vardenafil, tad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30
Inventor 周学敏汪洋吴小莉王舒王若愚吴金华
Owner NANJING MEDICAL UNIV
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