CN103604686A - Pre-treatment and quantitative analysis method for rapid determination of content of cadmium element in rice - Google Patents
Pre-treatment and quantitative analysis method for rapid determination of content of cadmium element in rice Download PDFInfo
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Abstract
The invention relates to a pre-treatment and quantitative analysis method for rapid determination of the content of the cadmium element in rice. The method comprises the following steps (1) crushing rice into powder; (2) preparing an agar solution with a concentration of 0.8 to 1.5 gL; (3) weighing a plurality of parts of rice powder as parallel samples, respectively subjecting the parallel samples to suspension and volume fixation with the agar solution prepared in the step (2), carrying out dilution with dilute nitric acid so as to obtain to-be-measured sample liquids with rice concentration of 4 to 16 gL and directly diluting the agar solution obtained in the step (2) with dilute nitric acid so as to obtain a blank sample; (4) preparing cadmium standard solutions, determining the absorbance value of each cadmium standard solution by using graphite furnace atomic absorption spectrometry and drafting a cadmium element standard curve; and (5) determining the absorbance values of the to-be-measured sample liquids and the blank sample and calculating cadmium content of the to-be-measured sample liquids. The method provided by the invention is simple and fast, can rapidly detect the content of the cadmium element in rice and has good accuracy and repeatability.
Description
Technical field
The invention belongs to express-analysis detection technique field, particularly pre-treatment and the quantitative analysis method of cadmium element content in a kind of Fast Measurement rice.
Background technology
In detecting rice, in the quantitative analysis method of cadmium element content, after conventionally the sample use acid after pulverizing need to being cleared up by pre-processing device, detect again.Conventional sample-pretreating method comprises: Wet, dry incineration, micro-wave digestion and high-pressure digestion tank are cleared up etc.In these methods, Wet need to consume a large amount of acid, and consuming time longer, and operation easier is large; Dry ashing needs first sample to be heated to charing, transfers to high temperature ashing in muffle furnace, and cooling rear acid adding is dissolved constant volume, and process is loaded down with trivial details and consuming time longer; High-pressure digestion tank is cleared up needs to utilize baking oven to the sample in tank and digestion solution heating and decompose, exists equally the problem of length consuming time; Micro-wave digestion adopts the mode of microwave heating to clear up sample, although compare several digestion procedures above, in pre-treatment speed, is enhanced, clear up and time of catching up with sour process to add up to need still in hour.Therefore, in traditional quantitative test rice, the pretreatment process of cadmium element is loaded down with trivial details, wastes time and energy, and loaded down with trivial details step is higher to testing staff's requirement, this has just caused the process length consuming time of whole quantitative analysis method, and operation is difficult, and the accuracy of result is also difficult to guarantee.
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 cadmium element content in a kind of Fast Measurement rice are provided, pre-treating method is simple and efficient, can fast detecting rice in cadmium element content, 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 cadmium element content 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 ~ 1.5 g/L;
(3) take some parts of rice powder of step (1) gained, as parallel sample, with step (2) gained agar solution constant volume, making the wherein concentration of rice is 10 ~ 40 g/L respectively, with rare nitric acid, dilute identical multiple, obtaining rice concentration is the sample liquid to be measured of 4 ~ 16 g/L;
The concentration that step (2) gained agar solution is directly made to agar solution with the dilution of rare nitric acid and sample liquid phase to be measured together, obtain sample blank;
(4) compound concentration is 0 ~ 10 ng/mL cadmium standard solution, adopts GFAAS (graphite furnace atomic absorption spectrometry) to measure the absorbance of each cadmium standard solution, take absorbance as ordinate, and concentration of standard solution is horizontal ordinate, obtains cadmium element typical curve;
(5) the described sample liquid to be measured of determination step (3) and the absorbance of sample blank, can obtain the cadmium content in sample liquid to be measured with both difference substitution cadmium element typical curve.
Press such scheme, described rice is any one in highed milled rice, rice germ or brown rice.
Press such scheme, the particle diameter after described rice is pulverized is not more than 40 orders.
Press such scheme, described in step (3), the volumetric concentration of rare nitric acid is 0.5 ~ 5%.
Press such scheme, while 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 and addition are all identical.
Press such scheme, in step (4), the concentration of palladium nitrate is 10 ~ 100 mg/L.
Press such scheme, agar solution described in step (2) can be hidden and preserve 4 ℃ of refrigerator and cooled, and one week interior with getting with use.
The present invention does not need to clear up sample, only rice powder need be made to the mode that Agar suspension can Spectroscopy With Suspension-injection and complete analysis during pre-treatment.Its principle is: powder diameter be not more than 40 object Rice Samples can be in certain density agar solution stable suspersion, after sample introduction, rice powder and agar solution can be removed at the ashing stage of heating schedule high temperature in graphite furnace, almost do not have matrix residual, the analysis of cadmium element can be do not disturbed, therefore the cadmium element content in rice can be analyzed fast and accurately.
Compared with prior art, the invention has the beneficial effects as follows:
(1) when the present invention measures cadmium element content, the pre-treatment of rice is not needed to clear up Rice Samples, the single Rice Samples pre-treatment time is no more than 3 min, operating process is easy fast, especially for a large amount of Rice Samples, saved a large amount of pre-treatment time, and the process of whole quantitative analysis method is also very short, swift to operate, the accuracy of result is high;
(2) in pretreatment process of the present invention, only used the rare nitric acid of very small amount of low concentration, method blank is low, environmentally friendly; And the acid that need to use a large amount of high concentrations with respect to methods such as Wets, neither need digestion process, do not need the acid treatment of catching up with before quantitative test yet;
(3) accuracy of method and repeatability are 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, the present invention is done to further detailed description, but working of an invention mode is not limited to this.
embodiment 1
The pre-treatment of cadmium element content and a quantitative analysis method in Fast Measurement rice, comprise following operation steps:
(1) brown rice after shelling is pulverized with flour mill, made coarse rice powder be placed in sealing bag all by 40 mesh sieves, mix, take 0.25 g sample in 25 mL color comparison tubes, take 6 parts of Duplicate Samples, numbering is respectively A ~ F;
(2) take 0.4 g agar powder in 1 L beaker, add and be slightly less than 500 mL ultrapure waters, heating is dissolved agar, standing cooling, mends and adds water to 500 mL, makes 0.8 g/L agar solution, standby;
(3) sample A ~ F is used respectively step (2) gained agar solution be settled to 25 mL, obtain respectively the suspending liquid of sample A ~ F, suspending liquid 0.6 mL of sample thief A ~ F, in 2 mL sample cups, with 2.5 times of 1% rare nitric acid dilutions, obtains Rice Samples A ~ F to be measured respectively; With same method, process Quality Control sample GBW10045, make quality-control sample Q;
Meanwhile, step (2) gained agar solution, directly with 2.5 times of 1% rare nitric acid dilutions, is made to sample blank;
(4) compound concentration is respectively 0,0.5,1.0,1.5,2.0, the cadmium element standard solution of 2.5 ng/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: detect wavelength 228.8 nm, slit width 0.7 nm, lamp current 8 mA, deuterium lamp method buckle back scape; C. use high-density graphite pipe, graphite furnace heating schedule is in Table 1;
(5) adopt same testing conditions, the absorbance of working sample blank, Rice Samples A ~ F to be measured and GBW10045 Quality Control sample Q, difference substitution step (4) the gained typical curve of Rice Samples and sample blank absorbance is calculated to the cadmium content in Rice Samples A ~ F, and the concentration value of the Quality Control sample Q calculating by same procedure and standard value are to the accuracy of definite method recently; Calculate the RSD value of 6 Duplicate Samples A ~ F testing results, with this, investigate the repeatability of method, concrete testing result is in Table 2.
(6) the concentration standard value of GBW10045 Quality Control sample Q is 0.19 ± 0.02 mg/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 3 min, and operating process is easy fast.
embodiment 2
The pre-treatment of cadmium element content and a quantitative analysis method in Fast Measurement rice, comprise following operation steps:
(1) brown rice after shelling is pulverized with flour mill, made coarse rice powder be placed in sealing bag all by 40 mesh sieves, mix, take 1.0 g samples in 25 mL color comparison tubes, take 6 parts of Duplicate Samples, numbering is respectively A ~ F;
(2) take 0.75 g agar powder in 1 L beaker, add and be slightly less than 500 mL ultrapure waters, heating is dissolved agar, standing cooling, mends and adds water to 500 mL, makes 1.5 g/L agar solutions, standby;
(3) sample A ~ F is settled to 25 mL with step (2) gained agar solution respectively, obtains respectively the suspending liquid of sample A ~ F; Suspending liquid 0.6 mL of sample thief A ~ F, in 2 mL sample cups, with 2.5 times of 1% rare nitric acid dilutions, obtains Rice Samples A ~ F to be measured respectively; With same method, process Quality Control sample GBW10045, make quality-control sample Q;
Meanwhile, step (2) gained agar solution, directly with 2.5 times of 1% rare nitric acid dilutions, is made to sample blank;
(4) compound concentration is respectively 0,1.0,1.5, the cadmium element standard solution of 2.0,2.5 ng/mL, absorbance with the standard solution of graphite furnace atomic absorption spectrometry variable concentrations cadmium, take concentration as horizontal ordinate, and 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 100 mg/L are as matrix modifier; B. instrument parameter is: detect wavelength 228.8 nm, slit width 0.7 nm, lamp current 8 mA, deuterium lamp method buckle back scape; C. use high-density graphite pipe, graphite furnace heating schedule is in Table 1;
(5) adopt same testing conditions, the absorbance of working sample blank, Rice Samples A ~ F to be measured and GBW10045 Quality Control sample Q, difference substitution step (4) the gained typical curve of Rice Samples and sample blank absorbance is calculated to the cadmium content in Rice Samples A ~ F, and the concentration value of the Quality Control sample Q calculating by same procedure and standard value are to the accuracy of definite method recently; Calculate the RSD value of 6 Duplicate Samples A ~ F testing results, with this, investigate the repeatability of method, concrete testing result is in Table 3.
(6) the concentration standard value of GBW10045 Quality Control sample Q is 0.19 ± 0.02 mg/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 3 min, and operating process is easy fast.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification made under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. pre-treatment and the quantitative analysis method of cadmium element content 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 ~ 1.5 g/L;
(3) take some parts of rice powder of step (1) gained, as parallel sample, with step (2) gained agar solution suspension constant volume, making the wherein concentration of rice is 10 ~ 40 g/L respectively, with rare nitric acid, dilute identical multiple, obtaining rice concentration is the sample liquid to be measured of 4 ~ 16 g/L;
Directly with rare nitric acid dilution, make the concentration of agar solution and sample liquid phase to be measured same step (2) gained agar solution, obtain sample blank;
(4) preparation cadmium standard solution, adopts GFAAS (graphite furnace atomic absorption spectrometry) to measure the absorbance of each cadmium standard solution, take absorbance as ordinate, and concentration of standard solution is horizontal ordinate, obtains cadmium element typical curve;
(5) the described sample liquid to be measured of determination step (3) and the absorbance of sample blank, can obtain the cadmium content in sample liquid to be measured with both difference substitution cadmium element typical curve.
2. pre-treatment and the quantitative analysis method of cadmium element content 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. pre-treatment and the quantitative analysis method of cadmium element content in a kind of Fast Measurement rice according to claim 1, is characterized in that: the particle diameter after described rice is pulverized is not more than 40 orders.
4. pre-treatment and the quantitative analysis method of cadmium element content in a kind of Fast Measurement rice according to claim 1, is characterized in that: described in step (3), the volumetric concentration of rare nitric acid is 0.5 ~ 5%.
5. pre-treatment and the quantitative analysis method of cadmium element content in a kind of Fast Measurement rice according to claim 1, it is characterized in that: while 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 and addition are all identical.
6. pre-treatment and the quantitative analysis method of cadmium element content in a kind of Fast Measurement rice according to claim 4, is characterized in that: in step (4), the concentration of palladium nitrate is 10 ~ 100 mg/L.
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| 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 |
| CN106290193A (en) * | 2016-08-18 | 2017-01-04 | 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 milk product |
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| CN110988099A (en) * | 2019-11-29 | 2020-04-10 | 黑龙江八一农垦大学 | Method for determining heavy metal elements in rice by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN106290193A (en) * | 2016-08-18 | 2017-01-04 | 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 milk product |
| 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 |
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| 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 | Method for determining heavy metal elements in rice by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
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