CN110389166A - The rapid detection method of heavy metal limit in a kind of food additives - Google Patents
The rapid detection method of heavy metal limit in a kind of food additives Download PDFInfo
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- CN110389166A CN110389166A CN201910775489.2A CN201910775489A CN110389166A CN 110389166 A CN110389166 A CN 110389166A CN 201910775489 A CN201910775489 A CN 201910775489A CN 110389166 A CN110389166 A CN 110389166A
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- G—PHYSICS
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- 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
- G01N1/38—Diluting, dispersing or mixing samples
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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
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Abstract
The embodiment of the invention provides a kind of rapid detection methods of heavy metal limit in food additives, include the following steps: step S1, sample pretreatment: the food additives sample of specified wt is weighed, sample is placed in conical flask and nitric acid solution is added, it is heated after placing preset time by electric hot plate, sulfuric acid solution is added after heating, adds nitric acid solution until the food additives sample decomposes complete, acquisition food additives sample solution；Machine in sampling: step S2 takes the food additives sample solution supernatant liquor filter membrane to analyze into sample injection bottle by inductivity coupled plasma mass spectrometry combined instrument；Step S3, standard solution are prepared: being taken lead standard solution, the lead standard solution is diluted with prescribed concentration nitric acid solution, to be configured to series standard working solution；Step S4, quantitative analysis: using lead content in inductivity coupled plasma mass spectrometry combined instrument measurement food additives sample solution and standard working solution, with signal response inner mark method ration.
Description
Technical field
The present invention relates to technical field of food additives, more particularly in a kind of food additives heavy metal limit it is fast
Fast detection method.
Background technique
Heavy metal includes the metallic elements such as lead, arsenic, mercury, chromium, cadmium, this dvielement is very difficult to be biodegradable, and can be
It is accumulated for a long time in organism, causes slow poisoning.
Heavy metal limit only has GB 5009.74-2014 " national food safety standard food additives in food additives
Middle heavy metal limit test ", this method Specimen eliminating carries out visual colorimetry with Na's colorimetry, in low-concentration heavy metal detection
When, colorimetric cylinder coloration determines that there are the risks of subjective bias, it is difficult to obtain reliable testing result.
Currently, for the detection of heavy metal limit in food additives, the not no test method of clear stipulaties.
Summary of the invention
In view of the above problems, it proposes the embodiment of the present invention and overcomes the above problem or at least partly in order to provide one kind
The rapid detection method of heavy metal limit in a kind of food additives to solve the above problems.
To solve the above-mentioned problems, the embodiment of the invention discloses a kind of quick inspections of heavy metal limit in food additives
Survey method, includes the following steps:
Step S1, sample pretreatment: weighing the food additives sample of specified wt, and sample is placed in conical flask and is added
Enter nitric acid solution, heated after placing preset time by electric hot plate, sulfuric acid solution is added after heating, add nitric acid solution up to
The food additives sample decomposes completely, obtains food additives sample solution；Machine in sampling: step S2 takes the food
Additive samples solution supernatant liquor filter membrane is analyzed into sample injection bottle by inductivity coupled plasma mass spectrometry combined instrument；Step
S3, standard solution are prepared: being taken lead standard solution, the lead standard solution is diluted with prescribed concentration nitric acid solution, to be configured to be
Column standard working solution；Quantitative analysis: step S4 measures food additives sample using inductivity coupled plasma mass spectrometry combined instrument
Lead content in product solution and standard working solution, with signal response inner mark method ration；
Further, the specified wt is 4.5~5.5g, and the preset time is 22~26h, and the conical flask is
25mL, the nitric acid solution are 5-15mL, and the sulfuric acid solution is 0-10mL；
Further, the step S2, comprising: food additives sample solution is cleared up, is added after clearing up sufficiently
The digestion solution of food additives sample is put into 50mL volumetric flask and carries out constant volume, takes supernatant liquor 10mL filter membrane by 20mL water
It is analyzed into sample injection bottle by inductivity coupled plasma mass spectrometry combined instrument；
Further, the step S3, comprising: standard solution is prepared: taking the 100mg/L lead standard solution of 0.5mL；Standard
Intermediate solution is prepared: being settled to 50mL to standard solution with 5% nitric acid solution, is configured to 1mg/L standard intermediate solution；Standard work
Make solution preparation: 5% nitric acid solution being used to distinguish dilution standard intermediate solution to 0.25,0.5,1,2,5,10 μ g/L as standard work
Make solution；
Further, the Mass Spectrometry Conditions of the inductivity coupled plasma mass spectrometry combined instrument are as follows:
Plasma flow amount: 14L/min；Carrier gas flux: 1.1L/min；Secondary air amount: 0.8L/min；Helium stream
Amount: 4mL/min~5mL/min；Atomization room temperature: 2 DEG C；Sample promotes rate: 0.3r/s；Atomizer: concentric atomizer；Sampling
Cone/interception cone: nickel cone；Analytical model: crash response pond；Detection mode: automatic；Number of repetition: 3；
Further, the detection formula of the quantitative analysis:
In formula, χ is the concentration of determinand in sample；C is the instrument readings of determinand in standard items；V is constant volume；f
For extension rate；M is sample weighting amount.
The embodiment of the present invention includes following advantages: having filled up the market vacancy, has met wanting for the client of this detection demand
It asks；Detection lower bound reaches 0.05mg/kg up to detection limit, and this method uses inductivity coupled plasma mass spectrometry combined instrument, avoids
Traditional visual colorimetry bring subjective bias.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is lead standard substance curve graph.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
The rapid detection method of heavy metal limit, includes the following steps: in a kind of food additives of the invention
Step S1, sample pretreatment: weighing the food additives sample of specified wt, and sample is placed in conical flask and is added
Enter nitric acid solution, heated after placing preset time by electric hot plate, sulfuric acid solution is added after heating, add nitric acid solution up to
The food additives sample decomposes completely, obtains food additives sample solution；
Machine in sampling: step S2 takes the food additives sample solution supernatant liquor filter membrane to pass through into sample injection bottle
The analysis of inductivity coupled plasma mass spectrometry combined instrument；
Step S3, standard solution are prepared: taking lead standard solution, it is molten to dilute the lead standard with prescribed concentration nitric acid solution
Liquid, to be configured to series standard working solution；
Quantitative analysis: step S4 measures food additives sample solution using inductivity coupled plasma mass spectrometry combined instrument
With lead content in standard working solution, with signal response inner mark method ration.
Wherein in step S1, the specified wt is 4.5~5.5g, and the preset time is 22~26h, the conical flask
For 25mL, the nitric acid solution is 5-15mL, and the sulfuric acid solution is 0-10mL.
Wherein in step S2, food additives sample solution is cleared up, 20mL water is added after clearing up sufficiently, by food
The digestion solution of additive samples is put into 50mL volumetric flask and carries out constant volume, and supernatant liquor 10mL filter membrane is taken to pass through into sample injection bottle
The analysis of inductivity coupled plasma mass spectrometry combined instrument.
Wherein in step S3, standard solution is prepared: taking the 100mg/L lead standard solution of 0.5mL；Standard intermediate solution is matched
System: 50mL is settled to standard solution with 5% nitric acid solution, is configured to 1mg/L standard intermediate solution；Standard working solution is matched
System: use 5% nitric acid solution difference dilution standard intermediate solution to 0.25,0.5,1,2,5,10 μ g/L as standard working solution.
Wherein in step S4, the Mass Spectrometry Conditions of the inductivity coupled plasma mass spectrometry combined instrument are as follows:
Plasma flow amount: 14L/min；Carrier gas flux: 1.1L/min；Secondary air amount: 0.8L/min；Helium stream
Amount: 4mL/min~5mL/min；Atomization room temperature: 2 DEG C；Sample promotes rate: 0.3r/s；Atomizer: concentric atomizer；Sampling
Cone/interception cone: nickel cone；Analytical model: crash response pond；Detection mode: automatic；Number of repetition: 3.
The detection formula of the quantitative analysis:
In formula, χ is the concentration of determinand in sample；C is the instrument readings of determinand in standard items；V is constant volume；f
For extension rate；M is sample weighting amount.
Embodiment one
The rapid detection method of heavy metal limit, includes the following steps: in a kind of food additives of the invention
Step S1, sample pretreatment: weighing the food additives sample of 5g, and sample is placed in 25mL conical flask and is added
10mL nitric acid solution, place for 24 hours afterwards by electric hot plate heat, after heating be added 5mL sulfuric acid solution, add nitric acid solution up to
The food additives sample decomposes completely, obtains food additives sample solution；
Machine in sampling: food additives sample solution is taken supernatant liquor 10mL filter membrane to lead into sample injection bottle by step S2
Cross the analysis of inductivity coupled plasma mass spectrometry combined instrument；
Step S3, standard solution are prepared: taking the 100mg/L lead standard solution of 0.5mL；Standard intermediate solution is prepared: with 5%
Nitric acid solution is settled to 50mL, is configured to 1mg/L standard intermediate solution；Standard working solution is prepared: being distinguished with 5% nitric acid solution
Dilution standard intermediate solution is to 0.25,0.5,1,2,5,10 μ g/L as standard working solution；
Step S4, quantitative analysis: using inductivity coupled plasma mass spectrometry combined instrument measurement sample solution and standard work
Lead content in solution, with signal response inner mark method ration.
Machine in sampling: food additives sample solution is taken supernatant liquor 10mL filter membrane to sample injection bottle by the step S2
In upper machine analysis process, comprising: food additives sample solution is cleared up, 20mL water is added after clearing up sufficiently, will eat
The digestion solution of product additive samples be put into 50mL volumetric flask carry out constant volume, take supernatant liquor 10mL filter membrane into sample injection bottle on
Machine analysis；
The Mass Spectrometry Conditions of the inductivity coupled plasma mass spectrometry combined instrument are as follows: plasma flow amount: 14L/min；
Carrier gas flux: 1.1L/min；Secondary air amount: 0.8L/min；Helium gas flow: 4mL/min~5mL/min；Atomization room temperature: 2
℃；Sample promotes rate: 0.3r/s；Atomizer: concentric atomizer；Sampling spiroid/interception cone: nickel cone；Analytical model: crash response
Pond；Detection mode: automatic；Number of repetition: 3.
Specifically, the food additives sample of weighing 5g is placed in 25mL conical flask, 10mL nitric acid is added, after placing for 24 hours
It is heated with electric hot plate, removes and let cool after reacting and mitigating, 5mL sulfuric acid is added along conical flask bottle wall, is further continued for being heated to conical flask
Solution begins to change into brown in bottle, and constantly dropwise addition nitric acid is complete to organic matter decomposition, continues to be heated to generating a large amount of titanium dioxide
Sulphur white smoke, last solution is in colourless or yellowish；20mL water is added after resolution sufficiently, after sufficiently catching up with acid, by digestion solution
The constant volume into 50mL volumetric flask；Take the upper machine analysis into sample injection bottle of supernatant liquor about 10mL filter membrane.
According to determining inductivity coupled plasma mass spectrometry condition measurement sample and standard working solution, response should all be
Within the range of linearity of instrument detection, with signal response inner mark method ration；The lead standard substance curve of the lead standard solution
Figure is shown referring to Fig.1, and standard substance response is shown in Table 1.
1 standard substance response of table
| BLANK | 48,982 |
| 0.25μg/L | 169,979 |
| 0.5μg/L | 321,222 |
| 1μg/L | 1,431,386 |
| 2μg/L | 2,804,107 |
| 5μg/L | 5,720,642 |
| 10μg/L | 15,381,699 |
2 sample test mean concentration of table
It is tested by the detection of sample and mark-on reclaims, detection limit reaches 0.05mg/kg.
Although the preferred embodiment of the embodiment of the present invention has been described, once a person skilled in the art knows bases
This creative concept, then additional changes and modifications can be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of range of embodiment of the invention.
Above to the rapid detection method of heavy metal limit in a kind of food additives provided by the present invention, carry out in detail
Thin to introduce, used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said
It is bright to be merely used to help understand method and its core concept of the invention；At the same time, for those skilled in the art, foundation
Thought of the invention, there will be changes in the specific implementation manner and application range, in conclusion the content of the present specification is not
It is interpreted as limitation of the present invention.
Claims (6)
1. the rapid detection method of heavy metal limit in a kind of food additives, which comprises the steps of:
Sample pretreatment: step S1 weighs the food additives sample of specified wt, sample is placed in conical flask and nitre is added
Acid solution is heated by electric hot plate after placing preset time, sulfuric acid solution is added after heating, adds nitric acid solution until described
Food additives sample decomposes completely, obtains food additives sample solution；
Machine in sampling: step S2 takes the food additives sample solution supernatant liquor filter membrane to pass through inductance into sample injection bottle
The analysis of coupled plasma mass spectrometry combined instrument；
Step S3, standard solution are prepared: lead standard solution taken, dilutes the lead standard solution with prescribed concentration nitric acid solution, with
It is configured to series standard working solution；
Step S4, quantitative analysis: using inductivity coupled plasma mass spectrometry combined instrument measurement food additives sample solution and mark
Lead content in quasi- working solution, with signal response inner mark method ration.
2. the rapid detection method of heavy metal limit in food additives according to claim 1, which is characterized in that described
Specified wt is 4.5~5.5g, and the preset time is 22~26h, and the conical flask is 25mL, and the nitric acid solution is 5-
15mL, the sulfuric acid solution are 0-10mL.
3. the rapid detection method of heavy metal limit in food additives according to claim 1, which is characterized in that described
Step S2, comprising:
Food additives sample solution is cleared up, 20mL water is added after clearing up sufficiently, by the resolution of food additives sample
Solution is put into 50mL volumetric flask and carries out constant volume, takes supernatant liquor 10mL filter membrane into sample injection bottle by inductively coupled plasma body
Mass spectrometer analysis.
4. the rapid detection method of heavy metal limit in food additives according to claim 1, which is characterized in that described
Step S3, comprising:
Standard solution is prepared: taking the 100mg/L lead standard solution of 0.5mL；Standard intermediate solution is prepared: with 5% nitric acid solution pair
Standard solution is settled to 50mL, is configured to 1mg/L standard intermediate solution；Standard working solution is prepared: being distinguished with 5% nitric acid solution
Dilution standard intermediate solution is to 0.25,0.5,1,2,5,10 μ g/L as standard working solution.
5. the rapid detection method of heavy metal limit in food additives according to claim 1, which is characterized in that described
The Mass Spectrometry Conditions of inductivity coupled plasma mass spectrometry combined instrument are as follows:
Plasma flow amount: 14L/min；Carrier gas flux: 1.1L/min；Secondary air amount: 0.8L/min；Helium gas flow:
4mL/min~5mL/min；Atomization room temperature: 2 DEG C；Sample promotes rate: 0.3r/s；Atomizer: concentric atomizer；Sampling spiroid/
Interception cone: nickel cone；Analytical model: crash response pond；Detection mode: automatic；Number of repetition: 3.
6. the rapid detection method of heavy metal limit in food additives according to claim 1, which is characterized in that described
The detection formula of quantitative analysis:
In formula, χ is the concentration of determinand in sample；C is the instrument readings of determinand in standard items；V is constant volume；F is dilute
Release multiple；M is sample weighting amount.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113916970A (en) * | 2021-08-31 | 2022-01-11 | 山东三星玉米产业科技有限公司 | Device and method for controlling heavy metal lead pollution risk in corn oil production |
| US11667992B2 (en) | 2021-07-19 | 2023-06-06 | Agilent Technologies, Inc. | Tip for interface cones |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080173806A1 (en) * | 2006-02-24 | 2008-07-24 | David Schneider | Saliva assay technique for heavy metal |
| CN105784827A (en) * | 2016-03-09 | 2016-07-20 | 广西壮族自治区环境监测中心站 | Method for measuring content of nine heavy metals in sugarcane juice with electric heating plate digestion/ICP-MS method |
| CN106093174A (en) * | 2016-05-30 | 2016-11-09 | 广西壮族自治区环境监测中心站 | The assay method of 7 heavy metal species content in a kind of heating board digestion/ICP MS method detection blackstrap |
| CN109297801A (en) * | 2018-11-09 | 2019-02-01 | 山东省食品药品检验研究院 | The detection method of arsenic in food additives silica |
| CN110018252A (en) * | 2019-04-10 | 2019-07-16 | 珠海天祥粤澳质量技术服务有限公司 | The detection method of 1,3,5- trichloro-benzenes in water quality |
-
2019
- 2019-08-21 CN CN201910775489.2A patent/CN110389166A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080173806A1 (en) * | 2006-02-24 | 2008-07-24 | David Schneider | Saliva assay technique for heavy metal |
| CN105784827A (en) * | 2016-03-09 | 2016-07-20 | 广西壮族自治区环境监测中心站 | Method for measuring content of nine heavy metals in sugarcane juice with electric heating plate digestion/ICP-MS method |
| CN106093174A (en) * | 2016-05-30 | 2016-11-09 | 广西壮族自治区环境监测中心站 | The assay method of 7 heavy metal species content in a kind of heating board digestion/ICP MS method detection blackstrap |
| CN109297801A (en) * | 2018-11-09 | 2019-02-01 | 山东省食品药品检验研究院 | The detection method of arsenic in food additives silica |
| CN110018252A (en) * | 2019-04-10 | 2019-07-16 | 珠海天祥粤澳质量技术服务有限公司 | The detection method of 1,3,5- trichloro-benzenes in water quality |
Non-Patent Citations (3)
| Title |
|---|
| 暨卫东: "《近海重金属污染元素监测与评价方法》", 31 August 2015, 海洋出版社 * |
| 杨立学: "电感耦合等离子体－质谱法测定婴幼儿食品中铅镉汞砷", 《现代预防医学》 * |
| 程敏: "口服液类保健食品中18种重金属元素检测", 《现代食品科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11667992B2 (en) | 2021-07-19 | 2023-06-06 | Agilent Technologies, Inc. | Tip for interface cones |
| CN113916970A (en) * | 2021-08-31 | 2022-01-11 | 山东三星玉米产业科技有限公司 | Device and method for controlling heavy metal lead pollution risk in corn oil production |
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