CN112379027A - Method for detecting melamine in soil - Google Patents
Method for detecting melamine in soil Download PDFInfo
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- CN112379027A CN112379027A CN202011168706.0A CN202011168706A CN112379027A CN 112379027 A CN112379027 A CN 112379027A CN 202011168706 A CN202011168706 A CN 202011168706A CN 112379027 A CN112379027 A CN 112379027A
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- methanol
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
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Abstract
The invention discloses a method for detecting melamine in soil, relates to the field of methods for detecting melamine in the field of environmental detection, and aims to solve the problem that a detection and analysis method is lacked when a specific industrial site is polluted by the substances. The method comprises the following steps: the method comprises the following steps: weighing a sample in a 50ml centrifuge tube; step two: adding 25ml of 1% trichloroacetic acid extracting solution, and fully shaking up; step three: adding 2ml of 2% acetic acid solution, and performing ultrasonic treatment for 20 min; step four: transferring part of the solution into a 10ml centrifuge tube, placing the centrifuge tube into a centrifuge, starting the centrifuge to enable the rotation speed to reach 8000rpn/min, and taking 3ml of supernatant to be purified; step five: activating and balancing a solid phase extraction column by taking 3ml of methanol and 3ml of water; step six: taking the supernatant, passing through a solid phase extraction column, and controlling the flow rate to be less than 0.5 ml/min; step seven: leaching the solid phase extraction column by using 3ml of water and 3ml of methanol; step eight: then eluting with 5ml of 5% ammoniated methanol; step nine: concentrating at 50 deg.C, blow drying, and diluting with 20% methanol/water to 2 ml; step ten: checking the performance of the high performance liquid chromatograph; step eleven: preparing a melamine standard curve solution; step twelve: and (5) carrying out sample injection analysis to obtain a determination result.
Description
Technical Field
The invention relates to the field of detection methods of melamine in soil in the field of environmental detection, in particular to a detection method of melamine in soil.
Background
In recent years, contamination of environmental media such as soil with melamine by various means has been reported. But the current detection method for melamine in soil and bottom mud at home and abroad is relatively blank, but has wide development prospect.
Therefore, the market urgently needs to develop a detection method of melamine in soil to help people to solve the existing problems.
Disclosure of Invention
The invention aims to provide a method for detecting melamine in soil, which aims to solve the problem that no method for detecting and analyzing the melamine in the soil exists in the national and environmental monitoring industries proposed in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for detecting melamine in soil comprises the following steps:
the method comprises the following steps: accurately weighing 2.5g (accurate to 0.001) of a sample in a 50ml centrifuge tube;
step two: adding 25ml of 1% trichloroacetic acid extracting solution, and fully shaking up;
step three: adding 2ml of 2% acetic acid solution, and performing ultrasonic treatment for 20 min;
step four: transferring part of the solution into a 10ml centrifuge tube, placing the centrifuge tube in a centrifuge, starting the centrifuge to enable the rotation speed to reach 8000rpn/min, and taking 3ml of supernatant after 10min to be purified;
step five: activating and balancing a solid phase extraction column by taking 3ml of methanol and 3ml of water;
step six: taking the supernatant, passing through a solid phase extraction column, and controlling the flow rate to be less than 0.5 ml/min;
step seven: leaching the solid phase extraction column by using 3ml of water and 3ml of methanol;
step eight: then eluting with 5ml of 5% ammoniated methanol;
step nine: concentrating at 50 deg.C, blow drying, and diluting with 20% methanol/water to 2 ml;
step ten: checking the performance of the high performance liquid chromatograph;
step eleven: preparing a melamine standard curve solution;
step twelve: and injecting the extract with constant volume into a high performance liquid chromatograph, analyzing by using a C18 column acetonitrile/water as a mobile phase, obtaining the concentration of the target analyte in the extract according to the established standard curve, and calculating the measurement result of the target analyte in the sample.
Preferably, in the first step, the drying temperature is 60 ℃, and the sample is sieved by a 60-mesh sieve;
preferably, in the second step, the volume ratio of the trichloroacetic acid solution used as the extracting solution is 1: 99.
Preferably, in the third step, the volume ratio of the acetic acid solution used is 2: 98.
Preferably, in the fourth step, the rotating speed of the centrifuge is 8000rpn/min, 10min or so.
Preferably, in the sixth step, the flow rate is controlled to be less than 0.5ml/min when solid phase extraction is used.
Preferably, in the ninth step, the mixture is dried by nitrogen at 50 ℃ and is made to 2ml by 20% methanol/water.
Preferably, in the eleventh step, the solvent used for preparing the standard solution is 20% methanol.
The invention has the beneficial effects that:
1. the method firstly determines the extraction, concentration, purification and measurement methods of the melamine in the soil;
2. the invention adopts a soil pretreatment method combining solid phase extraction and concentration, the efficiency is higher, and the pretreatment time of the sample can be controlled to be completed within 3-4 hours;
3. the invention adopts a high performance liquid phase measuring method, adopts a C18 column and uses acetonitrile/water as a mobile phase to measure the melamine, and has higher accuracy of measuring results.
Drawings
Fig. 1 is a working flow chart of a method for detecting melamine in soil according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, an embodiment of the present invention: a method for detecting melamine in soil comprises the following steps:
the method comprises the following steps: accurately weighing 2.5g (accurate to 0.001) of a sample in a 50ml centrifuge tube;
step two: adding 25ml of 1% trichloroacetic acid extracting solution, and fully shaking up;
step three: adding 2ml of 2% acetic acid solution, and performing ultrasonic treatment for 20 min;
step four: transferring part of the solution into a 10ml centrifuge tube, placing the centrifuge tube in a centrifuge, starting the centrifuge to enable the rotation speed to reach 8000rpn/min, and taking 3ml of supernatant after 10min to be purified;
step five: activating and balancing a solid phase extraction column by taking 3ml of methanol and 3ml of water;
step six: taking the supernatant, passing through a solid phase extraction column, and controlling the flow rate to be less than 0.5 ml/min;
step seven: leaching the solid phase extraction column by using 3ml of water and 3ml of methanol;
step eight: then eluting with 5ml of 5% ammoniated methanol;
step nine: concentrating at 50 deg.C, blow drying, and diluting with 20% methanol/water to 2 ml;
step ten: checking the performance of the high performance liquid chromatograph;
step eleven: preparing a melamine standard curve solution;
step twelve: and injecting the extract with constant volume into a high performance liquid chromatograph, analyzing by using a C18 column acetonitrile/water as a mobile phase, obtaining the concentration of the target analyte in the extract according to the established standard curve, and calculating the measurement result of the target analyte in the sample.
Further, in the first step, the drying temperature is 60 ℃, and the sample is sieved by a 60-mesh sieve;
further, in the second step, the volume ratio of the trichloroacetic acid solution used as the extracting solution is 1: 99.
Further, in the third step, the volume ratio of the acetic acid solution used is 2: 98.
Further, in the fourth step, the rotating speed of the centrifugal machine is 8000rpn/min, about 10 min.
Further, in the sixth step, the flow rate is controlled to be less than 0.5ml/min when solid phase extraction is used.
Further, in the ninth step, the mixture is dried by nitrogen at 50 ℃, and 20% methanol/water is used for fixing the volume to 2ml for testing.
Further, in the eleventh step, the solvent used for preparing the standard solution is 20% methanol.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A method for detecting melamine in soil is characterized by comprising the following steps:
the method comprises the following steps: accurately weighing 2.5g (accurate to 0.001) of a sample in a 50ml centrifuge tube;
step two: adding 25ml of 1% trichloroacetic acid extract, and fully shaking up;
step three: adding 2ml of 2% acetic acid solution, and performing ultrasonic treatment for 20 min;
step four: transferring part of the solution into a 10ml centrifuge tube, placing the centrifuge tube in a centrifuge, starting the centrifuge to enable the rotation speed to reach 8000rpn/min, and taking 3ml of supernatant after 10min to be purified;
step five: activating and balancing a solid phase extraction column by taking 3ml of methanol and 3ml of water;
step six: taking the supernatant, passing through a solid phase extraction column, and controlling the flow rate to be less than 0.5 ml/min;
step seven: leaching the solid phase extraction column by using 3ml of water and 3ml of methanol;
step eight: then eluting with 5ml of 5% ammoniated methanol;
step nine: concentrating at 50 deg.C, blow drying, and diluting with 20% methanol/water to 2 ml;
step ten: checking the performance of the high performance liquid chromatograph;
step eleven: preparing a melamine standard curve solution;
step twelve: and injecting the extract with constant volume into a high performance liquid chromatograph, analyzing by using a C18 column acetonitrile/water as a mobile phase, obtaining the concentration of the target analyte in the extract according to the established standard curve, and calculating the measurement result of the target analyte in the sample.
2. The method for detecting melamine in soil according to claim 1, wherein: in the first step, the drying temperature is 60 ℃, and the sample is sieved by a 60-mesh sieve.
3. The method for detecting melamine in soil according to claim 1, wherein: in the second step, the volume ratio of the adopted extract trichloroacetic acid solution is 1: 99.
4. the method for detecting melamine in soil according to claim 1, wherein: in the third step, the volume ratio of the acetic acid solution used is 2: 98.
5. The method for detecting melamine in soil according to claim 1, wherein: in the fourth step, the rotating speed of the centrifuge is 8000rpn/min, about 10 min.
6. The method for detecting melamine in soil according to claim 1, wherein: in the sixth step, the flow rate is controlled to be less than 0.5ml/min when solid phase extraction is used.
7. The method for detecting melamine in soil according to claim 1, wherein: in the ninth step, the mixture is dried by nitrogen at 50 ℃, and the volume is adjusted to 2ml by 20% methanol/water.
8. The method for detecting melamine in soil according to claim 1, wherein: in the eleventh step, the solvent used for preparing the standard solution is 20% methanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011168706.0A CN112379027A (en) | 2020-10-28 | 2020-10-28 | Method for detecting melamine in soil |
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| CN202011168706.0A CN112379027A (en) | 2020-10-28 | 2020-10-28 | Method for detecting melamine in soil |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048411A (en) * | 2012-08-06 | 2013-04-17 | 上海出入境检验检疫局工业品与原材料检测技术中心 | Pre-treating extraction method for detecting melamine in soil and fertilizer |
| CN105277634A (en) * | 2015-09-30 | 2016-01-27 | 中国兽医药品监察所 | Method for simultaneously and quantitatively detecting contents of melamine and cyanuric acid and application thereof |
| US20170115260A1 (en) * | 2015-03-09 | 2017-04-27 | Jiade Yu | Both Ultraviolet-Visible and Double Monochromatic Fluorescence Dual Detector for High Performance Liquid Chromatography |
| CN109490451A (en) * | 2018-10-16 | 2019-03-19 | 宁波中盛产品检测有限公司 | The universal precipitation and purification agent of strong water-soluble object and its pre-treating method of chromatography, Mass Spectrometer Method |
-
2020
- 2020-10-28 CN CN202011168706.0A patent/CN112379027A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048411A (en) * | 2012-08-06 | 2013-04-17 | 上海出入境检验检疫局工业品与原材料检测技术中心 | Pre-treating extraction method for detecting melamine in soil and fertilizer |
| US20170115260A1 (en) * | 2015-03-09 | 2017-04-27 | Jiade Yu | Both Ultraviolet-Visible and Double Monochromatic Fluorescence Dual Detector for High Performance Liquid Chromatography |
| CN105277634A (en) * | 2015-09-30 | 2016-01-27 | 中国兽医药品监察所 | Method for simultaneously and quantitatively detecting contents of melamine and cyanuric acid and application thereof |
| CN109490451A (en) * | 2018-10-16 | 2019-03-19 | 宁波中盛产品检测有限公司 | The universal precipitation and purification agent of strong water-soluble object and its pre-treating method of chromatography, Mass Spectrometer Method |
Non-Patent Citations (4)
| Title |
|---|
| YANFENG NONG 等: "A fast and low-cost method for determination of melamine in soil and sediment using high performance liquid chromatography", 《ANAL. METHODS》 * |
| 吴银良等: "气相色谱-质谱法测定土壤中三聚氰胺残留量", 《分析试验室》 * |
| 徐英江 等: "超高效液相色谱-串联质谱测定海水及沉积物中三聚氰胺", 《质谱学报》 * |
| 邱丰等: "固相萃取分离-离子色谱法测定化肥中三聚氰胺的含量", 《理化检验(化学分册)》 * |
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Application publication date: 20210219 |