CN114486472A - Pretreatment method for simultaneously determining multiple elements in agricultural products - Google Patents
Pretreatment method for simultaneously determining multiple elements in agricultural products Download PDFInfo
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- CN114486472A CN114486472A CN202210100793.9A CN202210100793A CN114486472A CN 114486472 A CN114486472 A CN 114486472A CN 202210100793 A CN202210100793 A CN 202210100793A CN 114486472 A CN114486472 A CN 114486472A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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Abstract
The invention discloses a pretreatment method for simultaneously measuring multiple elements in agricultural products, which is characterized by comprising the following steps of: step S1: preparing a sample: weighing a sample in a plastic centrifuge tube; step S2: adding a digestion solution: adding the acid system into a centrifuge tube filled with a sample; step S3: digestion: placing a centrifugal tube in S2 on a graphite digestion instrument for digestion, controlling the temperature at 100-140 ℃, taking out the centrifugal tube until 1mL of residual liquid is obtained, and obtaining a digestion solution, wherein the digestion time is controlled at 30-60 min; step S4: and (3) volume fixing: transferring the digestion solution in the S3 into a volumetric flask by using ultra-pure water, and performing constant volume to obtain a solution to be measured; step S5: and detecting the solution to be detected in S4. The invention can realize the simultaneous determination of five elements of copper, zinc, cadmium, lead and mercury, and has high digestion speed.
Description
Technical Field
The invention relates to the technical field of test analysis, in particular to a pretreatment method for simultaneously determining multiple elements in agricultural products.
Background
Along with the development of social process and industrialization process, industrial three wastes and town sewage are discharged randomly, crop irrigation water is often polluted, in addition, in order to improve the yield and quality of agricultural products, unreasonable phenomena also often occur in the use of chemical fertilizers, finally, heavy metals enter the environment for agricultural product growth, the quality of agricultural products is affected, and further, the health of people is affected. Therefore, the heavy metal detection of the agricultural products before entering the market is very important, and the pretreatment of the samples is very important in the heavy metal detection process of the agricultural product samples.
At present, the traditional pretreatment methods of agricultural product samples mainly comprise an electric heating plate digestion method, a pressure tank digestion method, a microwave digestion method and a reflux digestion method. The electric heating plate digestion method can cause loss of volatile elements (mercury), and the sample is easy to be polluted because acid needs to be continuously supplemented in the digestion process; the pressure tank digestion method needs to work in a high-pressure closed environment, and has long digestion time and slow determination speed; the microwave digestion method needs to buy special equipment, and the investment is large in the early stage, so that the microwave digestion method is not beneficial to technical popularization in a basic agricultural product detection mechanism; the reflux digestion method has complicated instrument and device, long digestion time and large reagent dosage, and is not suitable for measuring a large number of samples. In addition, mercury is a volatile element, and if the temperature is too high and the time is too long in the pretreatment process, the mercury can volatilize, and the temperature is too low and the time is short, other elements can be incompletely digested, so that simultaneous determination of multiple elements is difficult to realize.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a pretreatment method for simultaneously determining multiple elements in agricultural products.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a pretreatment method for simultaneously measuring a plurality of elements in agricultural products is characterized by comprising the following steps:
step S1: preparing a sample: weighing a sample in a plastic centrifuge tube;
step S2: adding a digestion solution: adding the acid system into a centrifuge tube filled with a sample;
step S3: digestion: placing a centrifugal tube in S2 on a graphite digestion instrument for digestion, controlling the temperature at 100-140 ℃, taking out the centrifugal tube until 1mL of residual liquid is obtained, and obtaining a digestion solution, wherein the digestion time is controlled at 30-60 min;
step S4: and (3) volume fixing: transferring the digestion solution in the S3 into a volumetric flask by using ultra-pure water, and performing constant volume to obtain a solution to be measured;
step S5: and detecting the solution to be detected in S4.
Further, 0.5g of the sample was weighed.
Further, the acid system is one of three different acid systems of nitric acid, nitric acid + hydrogen peroxide and nitric acid + perchloric acid.
Further, the amount of the acid system taken was 5 mL.
Further, the digestion temperature in the step S3 is controlled at 120 ℃, and the digestion time is controlled at 45-60 min.
Further, the volumetric flask in the step S4 is a 25mL volumetric flask.
Further, in step S5, an inductively coupled plasma mass spectrometer is used for detection.
Compared with the prior art, the invention has the following beneficial effects:
(1) the pretreatment method provided by the invention can realize complete digestion of mercury without causing volatilization of mercury, can realize simultaneous digestion and determination of five elements of copper, zinc, cadmium, lead and mercury, and has high digestion speed.
(2) The invention samples the standard sample to test, the measured value is in the range of the calibrated value, and the measuring precision is high.
(3) The method has simple operation steps and is suitable for the technical popularization of the detection mechanism of the basic agricultural products.
Detailed Description
The present invention is further illustrated by the following examples, which include, but are not limited to, the following examples.
The invention provides a pretreatment method for simultaneously measuring multiple elements in agricultural products, which comprises the following steps:
step S1: preparing a sample: weigh the sample into a plastic centrifuge tube.
Step S2: adding a digestion solution: adding the acid system into a centrifuge tube filled with a sample; here one of three different acid systems of nitric acid, nitric acid + hydrogen peroxide, nitric acid + perchloric acid.
Step S3: digestion: placing a centrifugal tube in S2 on a graphite digestion instrument for digestion, controlling the temperature at 100-140 ℃, taking out the centrifugal tube until 1mL of residual liquid is obtained, and obtaining a digestion solution, wherein the digestion time is controlled at 30-60 min;
the measurement instrument is damaged due to the fact that the acidity of the measurement solution is too high, the measurement environment is too complex due to the acidity, and measurement data are inaccurate, so that digestion liquid obtained after digestion under normal conditions can be detected only after acid removal, and the digestion liquid is taken out when being digested to 1mL, so that the acid removal is finished on the graphite digestion instrument, and the operation of taking out and carrying out independent acid removal is not needed.
Step S4: and (3) volume fixing: transferring the digestion solution in the S3 into a volumetric flask by using ultra-pure water, and performing constant volume to obtain a solution to be measured; when transferring the digested liquid after acid removal, care was taken to transfer the whole amount of the digested liquid to the volumetric flask.
Step S5: and detecting the solution to be detected in S4.
The first embodiment is as follows:
the embodiment provides a pretreatment method for simultaneously measuring multiple elements in agricultural products, which comprises the following steps:
step S1: preparing a sample: weighing 0.5g of standard rice sample of GBW10010(GSB-1) in a plastic centrifuge tube;
step S2: adding a digestion solution: adding 5mL of nitric acid and perchloric acid into a centrifuge tube filled with a sample, wherein the volume ratio of the nitric acid to the perchloric acid is 19: 1;
step S3: digestion: placing the centrifugal tube in the S2 on a graphite digestion instrument for digestion, wherein the digestion temperature is 120 ℃, and taking out the centrifugal tube when 1mL of liquid remains to obtain a digestion solution, and the digestion time is controlled to be 45-60 min;
step S4: and (3) volume fixing: transferring the digestion solution in the S3 into a 25mL volumetric flask by using ultra-pure water, and performing constant volume to obtain a solution to be measured;
step S5: detecting the solution to be detected in the S4 by using an atomic fluorescence spectrometer, wherein the detection result is shown in the following table:
table 1: content measurement value of each metal element in GBW10010(GSB-1) standard rice
| Metallic element | Measured value (mg/kg) | Calibration value (mg/kg) |
| Copper (Cu) | 4.670 | 4.9±0.3 |
| Zinc | 21.900 | 23±2 |
| Cadmium (Cd) | 0.088 | 0.087±0.005 |
| Lead (II) | 0.078 | 0.08±0.03 |
| Mercury | 0.0053 | 0.0053±0.0005 |
In this embodiment, the measured values of the five elements of copper, zinc, cadmium, lead and mercury are all within the range of calibration values.
Example two:
based on the first embodiment, the sample can also be selected from standard celery of GBW10048(GSB-26), and the detection result after digestion is shown in the following table:
table 2: content determination value of each metal element in standard celery of GBW10048(GSB-26)
| Metallic element | Measured value (mg/kg) | Calibration value (mg/kg) |
| Copper (Cu) | 7.83 | 8.2±0.4 |
| Zinc | 25.5 | 26±2 |
| Cadmium (Cd) | 0.089 | 0.092±0.006 |
| Lead (II) | 2.45 | 2.7±0.7 |
| Mercury | 0.0145 | 0.0146±0.0024 |
In this embodiment, the measured values of the five elements of copper, zinc, cadmium, lead and mercury are all within the range of calibration values.
The pretreatment method provided by the invention can realize complete digestion of mercury without causing volatilization of mercury, can realize simultaneous digestion and determination of five elements of copper, zinc, cadmium, lead and mercury, and has high digestion speed.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (7)
1. A pretreatment method for simultaneously measuring a plurality of elements in agricultural products is characterized by comprising the following steps:
step S1: preparing a sample: weighing a sample in a plastic centrifuge tube;
step S2: adding a digestion solution: adding the acid system into a centrifuge tube filled with a sample;
step S3: digestion: placing a centrifugal tube in S2 on a graphite digestion instrument for digestion, controlling the temperature at 100-140 ℃, taking out the centrifugal tube until 1mL of residual liquid is obtained, and obtaining a digestion solution, wherein the digestion time is controlled at 30-60 min;
step S4: and (3) volume fixing: transferring the digestion solution in the S3 into a volumetric flask by using ultra-pure water, and performing constant volume to obtain a solution to be measured;
step S5: and detecting the solution to be detected in S4.
2. The pretreatment method for simultaneously measuring multiple elements in agricultural products according to claim 1, wherein 0.5g of the sample is weighed.
3. The pretreatment method for simultaneously determining multiple elements in agricultural products according to claim 2, wherein the acid system is one of three different acid systems of nitric acid, nitric acid + hydrogen peroxide, nitric acid + perchloric acid.
4. The pretreatment method for simultaneously measuring multiple elements in agricultural products according to claim 3, wherein the amount of the acid system is 5 mL.
5. The pretreatment method for simultaneously measuring multiple elements in agricultural products according to claim 4, wherein the digestion temperature in the step S3 is controlled at 120 ℃, and the digestion time is controlled at 45-60 min.
6. The pretreatment method for simultaneously measuring multiple elements in agricultural products according to claim 5, wherein the volumetric flask in step S4 is a 25mL volumetric flask.
7. The pretreatment method for simultaneously measuring multiple elements in agricultural products according to claim 1 or 6, wherein in step S5, an inductively coupled plasma mass spectrometer is used for detection.
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| CN202210100793.9A CN114486472A (en) | 2022-01-27 | 2022-01-27 | Pretreatment method for simultaneously determining multiple elements in agricultural products |
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| CN202210100793.9A CN114486472A (en) | 2022-01-27 | 2022-01-27 | Pretreatment method for simultaneously determining multiple elements in agricultural products |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580330A (en) * | 2019-01-23 | 2019-04-05 | 刘益友 | A kind of method that batch measures cadmium, lead and arsenic in rice |
| CN110514510A (en) * | 2019-08-20 | 2019-11-29 | 重庆市农业科学院 | The digestion procedure of heavy metal in a kind of agricultural product |
| CN110987592A (en) * | 2019-12-31 | 2020-04-10 | 宁波市食品检验检测研究院 | Method for automatically and rapidly digesting food sample |
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- 2022-01-27 CN CN202210100793.9A patent/CN114486472A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580330A (en) * | 2019-01-23 | 2019-04-05 | 刘益友 | A kind of method that batch measures cadmium, lead and arsenic in rice |
| CN110514510A (en) * | 2019-08-20 | 2019-11-29 | 重庆市农业科学院 | The digestion procedure of heavy metal in a kind of agricultural product |
| CN110987592A (en) * | 2019-12-31 | 2020-04-10 | 宁波市食品检验检测研究院 | Method for automatically and rapidly digesting food sample |
Non-Patent Citations (4)
| Title |
|---|
| 徐卫华等: "快速消解技术—石墨炉法测定土壤及农产品中的镉含量", 《乡村科技》, pages 69 - 71 * |
| 曾勇等: "快速消解电感耦合等离子体质谱仪法测定大米粉中的铅与镉", 《安徽预防医学杂志》, vol. 26, no. 1, pages 8 - 11 * |
| 温韬等: "湿法快速消解-电感耦合等离子质谱法测定大米中的锌、铜、镍", 《食品安全质量检测学报》, vol. 11, no. 1, pages 209 - 214 * |
| 王欣美等: "快速湿法消解-电感耦合等离子体质谱法同时测定紫菜中铅、砷、汞、镉含量", 中国卫生检验杂志, no. 23, pages 2835 - 2837 * |
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