CN113655052B - 基于高活性MgO对四环素类抗生素可视化检测的方法 - Google Patents
基于高活性MgO对四环素类抗生素可视化检测的方法 Download PDFInfo
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- 229940072172 tetracycline antibiotic Drugs 0.000 title claims abstract description 38
- 230000000694 effects Effects 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 230000000007 visual effect Effects 0.000 title claims description 8
- 239000004098 Tetracycline Substances 0.000 claims abstract description 19
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 19
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 19
- 229960002180 tetracycline Drugs 0.000 claims abstract description 18
- 229930101283 tetracycline Natural products 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 230000000536 complexating effect Effects 0.000 claims abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 39
- 239000000395 magnesium oxide Substances 0.000 claims description 39
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 15
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 4
- 239000004100 Oxytetracycline Substances 0.000 claims description 3
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 claims description 3
- 229960004475 chlortetracycline Drugs 0.000 claims description 3
- CYDMQBQPVICBEU-XRNKAMNCSA-N chlortetracycline Chemical compound C1=CC(Cl)=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-XRNKAMNCSA-N 0.000 claims description 3
- 235000019365 chlortetracycline Nutrition 0.000 claims description 3
- 229960000625 oxytetracycline Drugs 0.000 claims description 3
- IWVCMVBTMGNXQD-PXOLEDIWSA-N oxytetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3[C@H](O)[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-PXOLEDIWSA-N 0.000 claims description 3
- 235000019366 oxytetracycline Nutrition 0.000 claims description 3
- IWVCMVBTMGNXQD-UHFFFAOYSA-N terramycin dehydrate Natural products C1=CC=C2C(O)(C)C3C(O)C4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000003086 colorant Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 241001465754 Metazoa Species 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 238000002965 ELISA Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 238000001917 fluorescence detection Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000001792 White test Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229940040944 tetracyclines Drugs 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
本发明提供一种用高活性MgO对四环素类抗生素可视化检测的方法。属于化学分析检测技术领域。将高活性MgO放入可能含有四环素类抗生素的水中，在可见光或者紫外光照射下，高活性MgO与四环素类抗生素发生络合反应，生成具有颜色的配合物，通过颜色的变化检测是否含有四环素，颜色越深，四环素类抗生素浓度越高。此外，通过离心干燥得到MgO粉末，与标准色卡比较颜色，能粗略分析四环素浓度。本发明利用高活性MgO，实现对四环素类抗生素简便、低成本和快速检测。
Description
技术领域
本发明属于化学分析检测技术领域，具体介绍了一种基于高活性MgO对四环素类抗生素可视化检测的方法。
背景技术
广谱抗生素中四环素类抗生素(主要包括金霉素、四环素和土霉素等)是目前使用最广泛，用量最大的抗生素之一。因其价格便宜抗菌效果好，广泛应用于医疗尤其是畜牧业当中。环境中四环素主要来源于医药企业排放的污水，因过期丢弃的药品、病人的新陈代谢以及农林畜牧业等。环境中高浓度四环素类抗生素对自然界、动物、植物和人类构成严重威胁。因此，开发一种价格低，无毒，有效、环保的对四环素类抗生素进行检测的方法，仍然是提供饮用水和环境保护的全球需求。
目前常见的四环素检测方法有：高效液相色谱法、液相-质谱联用法、微生物检测法，荧光检测法、免疫检测法，酶联免疫法和分光光度法等。其中高效液相色谱法、液相-质谱联用法和荧光检测法需要大型精密设备，价格昂贵，携带不方便。酶联免疫法和分光光度法交叉性强，容易被其他物质干扰，出现假阳性。因此，开发一种快速、简便、成本低的四环素类检测方法是很有必要的。
发明内容
本发明的目的是为了克服现有技术的缺陷而提供一种基于高活性MgO对四环素类抗生素可视化检测的方法。
本发明的目的是这样实现的：
一种基于高活性MgO对四环素类抗生素可视化检测的方法，包括如下步骤：
首先，将氧化镁在氢气/氩气气氛或者氩气气氛，高温500-900℃下活化2h～5h，得到高活性MgO粉末；
其次，将100mg高活性MgO投入到100mL可能含有四环素类抗生素的废水中，使用可见光或紫外光进行照射21-50分钟，促进高活性MgO和四环素发生络合反应，这时白色氧化镁颜色会发生变化，废水中四环素类抗生素浓度越高，MgO颜色越深，从而达到高活性MgO对四环素类抗生素的可视化检测。
所述四环素类抗生素为四环素、土霉素和金霉素中的一种或几种；
所述四环素类抗生素浓度为0-1000mg/L。
此外，将氧化镁负载到白色试纸上，即可制成四环素检测试纸。利用试纸表面MgO与四环素络合反应得到不同颜色的络合物，通过与标准色卡来对比，判断水中是否存在四环素并粗略分析四环素浓度。
与现有技术相比，本发明的有益效果是：
本发明高活性氧化镁能够与四环素快速发生显色络合反应。氧化镁价格便宜，无毒，来源丰富，经高温活化后，氧化镁表面容易暴露大量高活性的高活性镁，更容易与四环素发生配位反应。该方法具有操作简便、成本低、检测时间短、灵敏度高等优点，是一种非常有前景的抗生素检测方法。
附图说明
图1是镁与四环素类抗生素发生配位原理图；
图2(a)用高活性MgO检测0～50mg/L四环素后的粉末照片和(b)标准色卡。
具体实施方式
下面结合附图与具体实施方式对本发明作进一步详细描述。
实施方式一
本发明实施例1：定性检测水是否含有四环素类抗生素。取氧化镁在600℃下，氩气气氛中处理三个小时，得到高活性氧化镁。将0.1g上述产品放入到100mL可能含有四环素类抗生素的水中，使用300W氙灯进行照射30min。照射结束后，粉末由白色变为黄色或者棕色，则表示溶液含有四环素类抗生素，颜色越深，浓度越大。
实施方式二
本发明实施例2：粗略检测水中四环素类抗生素浓度。取氧化镁在600℃下，氩气气氛中处理三个小时，得到高活性氧化镁。将0.1g上述产品放入到100mL可能含有四环素类抗生素的水中，使用300W氙灯进行照射30min。照射结束后，将粉末离心，干燥。将干燥好的MgO粉末与我们提供标椎色卡进行对比，可以粗略定量四环素类抗生素浓度。
本发明公开了一种用高活性MgO对四环素类抗生素可视化检测的方法。属于化学分析检测技术领域。将高活性MgO放入可能含有四环素类抗生素的水中，在可见光或者紫外光照射下，高活性MgO与四环素类抗生素发生络合反应，生成具有颜色的配合物，通过颜色的变化检测是否含有四环素，颜色越深，四环素类抗生素浓度越高。此外，通过离心干燥得到MgO粉末，与标准色卡比较颜色，能粗略分析四环素浓度。本发明利用高活性MgO，实现对四环素类抗生素简便、低成本和快速检测。
Claims (3)
1.一种基于高活性MgO对四环素类抗生素可视化检测的方法，其特征在于：包括如下步骤：
首先，将氧化镁在氢气/氩气气氛或者氩气气氛，高温500-900℃下活化2h～5h，得到高活性MgO粉末；
其次，将100mg高活性MgO投入到100mL可能含有四环素类抗生素的废水中，使用可见光或紫外光进行照射21-50分钟，促进高活性MgO和四环素发生络合反应，这时白色氧化镁颜色会发生变化，废水中四环素类抗生素浓度越高，MgO颜色越深，从而达到高活性MgO对四环素类抗生素的可视化检测。
2.根据权利要求1所述的基于高活性MgO对四环素类抗生素可视化检测的方法，其特征在于：所述四环素类抗生素为四环素、土霉素和金霉素中的一种或几种。
3.根据权利要求1所述的基于高活性MgO对四环素类抗生素可视化检测的方法，其特征在于：所述四环素类抗生素浓度为0-1000mg/L。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4126680A (en) * | 1977-04-27 | 1978-11-21 | Pfizer Inc. | Tetracycline antibiotic compositions |
| EP0271374A2 (fr) * | 1986-12-10 | 1988-06-15 | So.Ge.Val S.A. | Composition antibiotique aqueuse à usage vétérinaire |
| CN103033502A (zh) * | 2012-11-16 | 2013-04-10 | 陕西理工学院 | 一种鸡蛋清中残留土霉素药品的快速检测方法 |
| CN107064040A (zh) * | 2017-06-23 | 2017-08-18 | 江苏省环境科学研究院 | 水环境中痕量抗生素的高效富集与分离方法 |
| CN107159094A (zh) * | 2017-05-26 | 2017-09-15 | 湖南农业大学 | 磁性氢氧化镁吸附剂去除废水中四环素的方法 |
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2021
- 2021-08-03 CN CN202110887308.2A patent/CN113655052B/zh active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4126680A (en) * | 1977-04-27 | 1978-11-21 | Pfizer Inc. | Tetracycline antibiotic compositions |
| EP0271374A2 (fr) * | 1986-12-10 | 1988-06-15 | So.Ge.Val S.A. | Composition antibiotique aqueuse à usage vétérinaire |
| CN103033502A (zh) * | 2012-11-16 | 2013-04-10 | 陕西理工学院 | 一种鸡蛋清中残留土霉素药品的快速检测方法 |
| CN107159094A (zh) * | 2017-05-26 | 2017-09-15 | 湖南农业大学 | 磁性氢氧化镁吸附剂去除废水中四环素的方法 |
| CN107064040A (zh) * | 2017-06-23 | 2017-08-18 | 江苏省环境科学研究院 | 水环境中痕量抗生素的高效富集与分离方法 |
Non-Patent Citations (3)
| Title |
|---|
| In-situ growth of magnesium peroxide on the edge of magnesium oxide nanosheets: Ultrahigh photocatalytic efficiency based on synergistic catalysis;Wenjing Zeng 等;Journal of Colloid and Interface Science;第561卷;第257–264页 * |
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