CN103604686B - The pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice - Google Patents
The pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice Download PDFInfo
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Abstract
The present invention relates to pre-treatment and the quantitative analysis method of rapid determination of content of cadmium element in a kind of Fast Measurement rice, it comprises the following steps: rice is ground into powder by (1); (2) compound concentration is the agar solution of 0.8 ~ 1.5g/L; (3) take the some parts of rice powder as parallel sample, respectively with step (2) gained agar solution suspension constant volume, and with dust technology dilution, obtain the sample liquid to be measured that rice concentration is 4 ~ 16g/L; By step (2) gained agar solution directly with dust technology dilution, obtain sample blank; (4) prepare cadmium standard solution, adopt GFAAS (graphite furnace atomic absorption spectrometry) to measure the absorbance of each cadmium standard solution, draw cadmium element typical curve; (5) absorbance of working sample liquid to be measured and sample blank, the cadmium content in calculation sample liquid to be measured.Pre-treating method of the present invention is simple and efficient, can detect rapid determination of content of cadmium element in rice fast, simultaneously accuracy and reproducible.
Description
Technical field
The invention belongs to express-analysis detection technique field, the particularly pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice.
Background technology
In the quantitative analysis method detecting rapid determination of content of cadmium element in rice, detect again after usually needing the sample after by pulverizing to use acid to clear up by pre-processing device.Conventional sample-pretreating method comprises: Wet, dry incineration, micro-wave digestion and high-pressure digestion tank are cleared up.In these methods, Wet needs to consume a large amount of acid, and consuming time longer, and operation easier is large; Dry ashing needs first by sample heating charing, and transfer in muffle furnace high temperature ashing, add acid dissolve constant volume after cooling, process is loaded down with trivial details and consuming time longer; High-pressure digestion tank is cleared up, and needs to utilize baking oven to the sample in tank and digestion solution heating and decompose, there is the problem of length consuming time equally; Micro-wave digestion adopts the mode of microwave heating to clear up sample, is enhanced in pre-treatment speed although compare several digestion procedure above, clear up and time of catching up with sour process to add up to need still in hour.Therefore, the pretreatment process that traditional quantitative analyzes cadmium element in rice is loaded down with trivial details, wastes time and energy, and the requirement of loaded down with trivial details step to testing staff is higher, this just causes the process length consuming time of whole quantitative analysis method, and operation is difficult, and the accuracy of result is also difficult to ensure.
Summary of the invention
Technical matters to be solved by this invention is for above-mentioned deficiency of the prior art, pre-treatment and the quantitative analysis method of rapid determination of content of cadmium element in a kind of Fast Measurement rice are provided, pre-treating method is simple and efficient, can detect rapid determination of content of cadmium element in rice fast, simultaneously accuracy and reproducible.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows:
The pre-treatment of rapid determination of content of cadmium element and a quantitative analysis method in Fast Measurement rice, comprise following operation steps:
(1) rice is ground into powder;
(2) agar powder heating for dissolving in ultrapure water, is mixed with the agar solution that concentration is 0.8 ~ 1.5g/L;
(3) some parts of rice powder of step (1) gained are taken, as parallel sample, respectively with step (2) gained agar solution constant volume, the concentration of wherein rice is made to be 10 ~ 40g/L, dilute identical multiple with dust technology, obtain the sample liquid to be measured that rice concentration is 4 ~ 16g/L;
Step (2) gained agar solution is directly made the concentration of agar solution and sample liquid phase to be measured together with dust technology dilution, obtains sample blank;
(4) compound concentration is 0 ~ 10ng/mL cadmium standard solution, and adopt GFAAS (graphite furnace atomic absorption spectrometry) to measure the absorbance of each cadmium standard solution, take absorbance as ordinate, concentration of standard solution is horizontal ordinate, obtains cadmium element typical curve;
(5) the sample liquid to be measured described in determination step (3) and the absorbance of sample blank, can obtain the cadmium content in sample liquid to be measured with both differences substitution cadmium element typical curve.
By such scheme, described rice is any one in highed milled rice, rice germ or brown rice.
By such scheme, the particle diameter after described rice pulverizing is not more than 40 orders.
By such scheme, described in step (3), the volumetric concentration of dust technology is 0.5 ~ 5%.
By such scheme, when adopting GFAAS (graphite furnace atomic absorption spectrometry) to measure absorbance in step (4) and step (5), also add palladium nitrate as matrix modifier, the concentration of matrix modifier is all identical with addition.
By such scheme, in step (4), the concentration of palladium nitrate is 10 ~ 100mg/L.
By such scheme, agar solution described in step (2) can be hidden 4 DEG C of refrigerator and cooled and preserve, one week interior with get with.
The present invention does not need to clear up sample, only rice powder need be made Agar suspension and the mode of Spectroscopy With Suspension-injection can complete analysis during pre-treatment.Its principle is: powder diameter be not more than 40 object Rice Samples can in certain density agar solution stable suspersion, after sample introduction, rice powder and agar solution can be removed at the ashing stage high temperature of heating schedule in graphite furnace, matrix is not almost had to remain, the analysis of cadmium element can not be disturbed, therefore can analyze the rapid determination of content of cadmium element in rice fast and accurately.
Compared with prior art, the invention has the beneficial effects as follows:
(1) when the present invention measures rapid determination of content of cadmium element, do not need to clear up Rice Samples to the pre-treatment of rice, the single Rice Samples pre-treatment time is no more than 3min, operating process is fast easy, especially a large amount of pre-treatment time is saved for a large amount of Rice Samples, and the process of whole quantitative analysis method is also very short, swift to operate, the accuracy of result is high;
(2) only used very small amount of low concentration dust technology in pretreatment process of the present invention, method blank is low, environmentally friendly; And need the acid of using a large amount of high concentration relative to methods such as Wets, neither need digestion process, before also not needing quantitative test, catch up with acid treatment;
(3) accuracy of method and repeatability good;
(4) agar powder is cheap and easy to get, and environmentally safe.
Accompanying drawing explanation
Fig. 1 is cadmium element typical curve in embodiment 1.
Fig. 2 is cadmium element typical curve in embodiment 2.
Embodiment
Below in conjunction with embodiment, further detailed description is done to the present invention, but working of an invention mode is not limited thereto.
Embodiment 1
The pre-treatment of rapid determination of content of cadmium element and a quantitative analysis method in Fast Measurement rice, comprise following operation steps:
(1) pulverized with flour mill by the brown rice after shelling, make coarse rice powder all by 40 mesh sieves, can be placed in sealing bag, mixing, takes 0.25g sample in 25mL color comparison tube, takes 6 parts of Duplicate Samples, and numbering is respectively A ~ F;
(2) take 0.4g agar powder in 1L beaker, add and be slightly less than 500mL ultrapure water, heating makes agar dissolve, and leaves standstill cooling, mends and adds water to 500mL, obtained 0.8g/L agar solution, for subsequent use;
(3) step (2) gained agar solution is used by sample A ~ F to be settled to 25mL respectively, obtain the suspending liquid of sample A ~ F respectively, the suspending liquid 0.6mL of sample thief A ~ F is in 2mL sample cup respectively, dilutes 2.5 times, obtain Rice Samples A ~ F to be measured with 1% dust technology; Process Quality Control sample GBW10045 in the same way, obtained quality-control sample Q;
Meanwhile, step (2) gained agar solution is directly diluted 2.5 times with 1% dust technology, obtained sample blank;
(4) compound concentration is respectively 0,0.5,1.0,1.5,2.0, the cadmium element standard solution of 2.5ng/mL, with the absorbance of the standard solution of graphite furnace atomic absorption spectrometry variable concentrations cadmium, take concentration as horizontal ordinate, absorbance is ordinate, record cadmium element typical curve (see figure 1), Abs=0.092691Conc+0.068857, r=0.9990;
Condition determination comprises: a. adopts automatic sampler sample introduction, and cadmium element standard solution sample size is 10 μ L; B. instrument parameter is: determined wavelength 228.8nm, slit width 0.7nm, lamp current 8mA, deuterium lamp method buckle back scape; C. use high-density graphite pipe, graphite furnace heating schedule is in table 1;
(5) same testing conditions is adopted, working sample is blank, the absorbance of Rice Samples A ~ F to be measured and GBW10045 Quality Control sample Q, the difference of Rice Samples and sample blank absorbance is substituted into step (4) gained typical curve and calculate cadmium content in Rice Samples A ~ F, and the concentration value of the Quality Control sample Q calculated by same procedure and standard value contrast the accuracy carrying out defining method; Calculate the RSD value of 6 Duplicate Samples A ~ F testing results, investigate the repeatability of method with this, concrete testing result is in table 2.
(6) the concentration standard value of GBW10045 Quality Control sample Q is 0.19 ± 0.02mg/kg, and this method acquired results and standard value meet, and illustrates that this method accuracy is good; 6 Duplicate Samples measurement result RSD are 3.7%, illustrate that this method has good repeatability;
(7) each time for sample pretreatment of this method is all no more than 3min, and operating process is fast easy.
Embodiment 2
The pre-treatment of rapid determination of content of cadmium element and a quantitative analysis method in Fast Measurement rice, comprise following operation steps:
(1) pulverized with flour mill by the brown rice after shelling, make coarse rice powder all by 40 mesh sieves, can be placed in sealing bag, mixing, takes 1.0g sample in 25mL color comparison tube, takes 6 parts of Duplicate Samples, and numbering is respectively A ~ F;
(2) take 0.75g agar powder in 1L beaker, add and be slightly less than 500mL ultrapure water, heating makes agar dissolve, and leaves standstill cooling, mends and adds water to 500mL, obtained 1.5g/L agar solution, for subsequent use;
(3) sample A ~ F is settled to 25mL with step (2) gained agar solution respectively, obtains the suspending liquid of sample A ~ F respectively; The suspending liquid 0.6mL of sample thief A ~ F is in 2mL sample cup respectively, dilutes 2.5 times, obtain Rice Samples A ~ F to be measured with 1% dust technology; Process Quality Control sample GBW10045 in the same way, obtained quality-control sample Q;
Meanwhile, step (2) gained agar solution is directly diluted 2.5 times with 1% dust technology, obtained sample blank;
(4) compound concentration is respectively 0,1.0, the cadmium element standard solution of 1.5,2.0,2.5ng/mL, with the absorbance of the standard solution of graphite furnace atomic absorption spectrometry variable concentrations cadmium, take concentration as horizontal ordinate, absorbance is ordinate, records cadmium element typical curve (see figure 2), Abs=0.14851Conc+0.084649, r=0.9988;
Condition determination comprises: a. adopts automatic sampler sample introduction, and cadmium element standard solution sample size is 10 μ L, and to add concentration be that the palladium nitrate solution 5 μ L of 100mg/L is as matrix modifier; B. instrument parameter is: determined wavelength 228.8nm, slit width 0.7nm, lamp current 8mA, deuterium lamp method buckle back scape; C. use high-density graphite pipe, graphite furnace heating schedule is in table 1;
(5) same testing conditions is adopted, working sample is blank, the absorbance of Rice Samples A ~ F to be measured and GBW10045 Quality Control sample Q, the difference of Rice Samples and sample blank absorbance is substituted into step (4) gained typical curve and calculate cadmium content in Rice Samples A ~ F, and the concentration value of the Quality Control sample Q calculated by same procedure and standard value contrast the accuracy carrying out defining method; Calculate the RSD value of 6 Duplicate Samples A ~ F testing results, investigate the repeatability of method with this, concrete testing result is in table 3.
(6) the concentration standard value of GBW10045 Quality Control sample Q is 0.19 ± 0.02mg/kg, and this method acquired results and standard value meet, and illustrates that this method accuracy is good; 6 Duplicate Samples measurement result RSD are 3.41%, illustrate that this method has good repeatability;
(7) each time for sample pretreatment of this method is all no more than 3min, and operating process is fast easy.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification made under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. the pre-treatment of rapid determination of content of cadmium element and a quantitative analysis method in Fast Measurement rice, is characterized in that: comprise following operation steps:
(1) rice is ground into powder;
(2) agar powder heating for dissolving in ultrapure water, is mixed with the agar solution that concentration is 0.8 ~ 1.5g/L;
(3) some parts of rice powder of step (1) gained are taken, as parallel sample, respectively with step (2) gained agar solution suspension constant volume, the concentration of wherein rice is made to be 10 ~ 40g/L, dilute identical multiple with dust technology, obtain the sample liquid to be measured that rice concentration is 4 ~ 16g/L;
By step (2) gained agar solution directly with dust technology dilution, make the concentration of agar solution and sample liquid phase to be measured together, obtain sample blank;
(4) prepare cadmium standard solution, adopt GFAAS (graphite furnace atomic absorption spectrometry) to measure the absorbance of each cadmium standard solution, take absorbance as ordinate, concentration of standard solution is horizontal ordinate, obtains cadmium element typical curve;
(5) the sample liquid to be measured described in determination step (3) and the absorbance of sample blank, can obtain the cadmium content in sample liquid to be measured with both differences substitution cadmium element typical curve.
2. the pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice according to claim 1, is characterized in that: described rice is any one in highed milled rice, rice germ or brown rice.
3. the pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice according to claim 1, is characterized in that: described rice pulverize after particle diameter be not more than 40 orders.
4. the pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice according to claim 1, is characterized in that: described in step (3), the volumetric concentration of dust technology is 0.5 ~ 5%.
5. the pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice according to claim 1, it is characterized in that: when adopting GFAAS (graphite furnace atomic absorption spectrometry) to measure absorbance in step (4) and step (5), also add palladium nitrate as matrix modifier, the concentration of matrix modifier is all identical with addition.
6. the pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice according to claim 5, is characterized in that: in step (4), the concentration of palladium nitrate is 10 ~ 100mg/L.
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| CN104897594A (en) * | 2015-05-13 | 2015-09-09 | 中国农业大学 | Method used for determining nano-silver content of bean sprout |
| CN105651543A (en) * | 2016-01-20 | 2016-06-08 | 山东科技大学 | Determination method for chromium content of inhalable particles in soil dust and detection method |
| CN106290193B (en) * | 2016-08-18 | 2019-01-18 | 浙江华才检测技术有限公司 | A kind of direct injected quickly measures the analysis method of cadmium content in dairy products |
| CN107884468A (en) * | 2017-11-29 | 2018-04-06 | 华中农业大学 | Application of the rice grain trace element in identification ratooning rice first rice crop rice and regeneration season rice |
| CN110274882A (en) * | 2018-03-16 | 2019-09-24 | 福建省农业科学院农业质量标准与检测技术研究所 | Cadmium detrmination method in rice |
| CN109580330A (en) * | 2019-01-23 | 2019-04-05 | 刘益友 | A kind of method that batch measures cadmium, lead and arsenic in rice |
| CN110988099A (en) * | 2019-11-29 | 2020-04-10 | 黑龙江八一农垦大学 | A method for the determination of heavy metal elements in rice by ICP-MS |
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