CN104122241A - Method for rapid determination of selenium content in tetrastigmatis hemsleyani - Google Patents
Method for rapid determination of selenium content in tetrastigmatis hemsleyani Download PDFInfo
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Abstract
The invention discloses a method for rapid determination of the selenium content in tetrastigmatis hemsleyani, wherein a microwave digestion-hydride generation-atomic fluorescence spectrometry method is adopted for determination of the selenium content. With microwave digestion, the digestion efficiency is high and fast, moreover, acid removing is not required after digestion, operation steps are simplified, pollution is reduced, the accuracy rate is increased, disadvantages of easy pollution of wet digestion and long digestion time are avoided, acid removing is not required, concentrated hydrochloric acid is directly added for reduction of selenium, and the digestion procedures are simplified; the detection cycle is greatly shortened, and the original detection cycle of 8-10 hours is shortened to 2-3 hours; and the detection is rapid and accurate, and the operation is simple.
Description
Technical field
The invention belongs to physical and chemical inspection field, specifically a kind of method of Se content in Fast Measurement radix tetrastigme.
Background technology
Radix tetrastigme (Tetrastigmatis hemsleyani), has another name called: having angle Japanese Cayratia Herb, stone mouse, is Vitaceae Tetrastigma plant, and its piece root is called hemsley rockvine root.Radix tetrastigme is mainly distributed in the Changjiang river areas to the south, be born in the other sylvan life of dark and damp hillside, gully or trench, with piece root or herb people medicine, for Guangxi conventional Chinese herbal medicine among the people, have antiviral, anti-inflammatory, analgesia and antipyretic, the effect such as protect the liver, and spinoff is little, be " bouvardin " that Western medicine cannot replace.Recent study is found, radix tetrastigme ethyl acetate extract is the most effective composition of antitumor common drug, its not only can slow down growth of cancer cell, and liver cancer and blood cell strain had to " apoptosis-promoting effect ", this important discovery has greatly promoted its using value and prospect medically.The Chinese patent drug that at present radix tetrastigme is used to the types such as antitumor, antirheumatic, hepatitis processed is produced, as radix tetrastigme particle, golden stilbene sheet, spun gold first capsule, Huatuo's rheumatism health-care capsule etc.The diseases such as anticancer and anti AIDS virus, antitumor, treatment blood disease and cardiovascular and cerebrovascular disease, hepatitis, meningitis, acute bronchitis, pneumonia, enteritis and sphagitis, infantile hyperpyrexia caused by exogenous pathogenic factor are widely used in clinically.
Selenium element is one of trace element of needed by human, endemic disease, various cancer, angiocardiopathy, complement activation and Hemorrhagic fever, male sterility and forepart pregnant women hypertension, radiation damage, the body reparation that Keshan disease, Kaschin-Beck disease and iodine deficiency are relevant and delay senility, immunologic function and acquired immune deficiency syndrome (AIDS), heavy metal toxicity and occupational illness etc. all closely related with selenium.Selenium is the activated centre of glutathione peroxidase (GSH-Px).Have anti-cancer, anticancer, anti-oxidant, prevent multiple endemic illness, antagonism toxic heavy metal, strengthen body immunity, delay senility, protect liver and the effect such as cardiac muscle is healthy.
To concentrate on and do hypertension drug, anti-inflammatory drug, cancer therapy drug three broad aspect containing selenium drug main in the world.Radix tetrastigme is as one for cancer therapy drug, and Se content research is essential.
At present, the assay method of selenium mainly contains: atomic absorption spectrography (AAS), inductively coupled plasma mass spectrometry, ultraviolet spectrophotometry, electrochemical methods, By Naa and By Hydride Generation-atomic Fluorescence Spectrometry.In these methods, By Hydride Generation-atomic Fluorescence Spectrometry has the advantages such as detection limit is low, spectrum disturbs less, chemistry interference is low, the range of linearity is wide, easy and simple to handle, operating cost is low.
The method of the existing disclosed hydride generation-AFS DETERMINATION of document Se content.As " mensuration of dietary Se " (GB/T13883-2008), " detection method of tealeaves leaf Se content " (GB/T21729-2008), " mensuration (GB5009.93-2010) of national food safety standard selenium in food etc., said method all adopts Wet, complicated operation; While using micro-wave digestion, need catch up with acid treatment, the cycle of clearing up is long; And in mensuration process, all used hydrochloric acid solution and the potassium ferricyanide solution of 6mol/L, reagent dosage is large, complicated operation.
The method of disclosed employing hydride generation-AFS DETERMINATION Se content has: number of patent application is the method that 20111027682.0,201110427886.4 and 201110427880.7 Chinese patent application discloses respectively Fast Measurement plant sample, animal tissue and Selenium in Soils content, all adopt nitric acid-perchloric acid acid mixture Wet, hydride generation-AFS DETERMINATION, but Wet program is loaded down with trivial details, complicated operation, error is large.
There is the shortcoming such as complicated operation or determination period length in the method existing at present.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of simple to operate, method of Se content in Fast Measurement radix tetrastigme accurately.
To achieve these goals, technical scheme of the present invention is as follows:
A method for Se content in Fast Measurement radix tetrastigme, comprises the following steps:
(1) micro-wave digestion: use nitric acid to carry out micro-wave digestion processing to radix tetrastigme sample; Described micro-wave digestion is undertaken by microwave dissolver program, after having cleared up, is that 30-45% hydrochloric acid reduces to radix tetrastigme sample by volumetric concentration, and constant volume obtains sample solution, for subsequent use; Prepare blank sample simultaneously, for subsequent use;
(2) drawing standard curve and set up regression equation: be mixed with the selenium standard solution of concentration gradient as 0-20 μ g/L taking selenium national standard solution as mother liquor, adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, according to the measurement result drawing standard curve of selenium standard solution and set up regression equation;
(3) measure and calculation: blank sample and sample solution are measured by hydride generation-atomic fluorescence spectrometer; Obtain the content of Selenium In Some Selenium-rich Biological Samples according to formula (I):
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
The program of clearing up of the micro-wave digestion described in above step (1) is: power is permanent is 1600W, first from 5min to 120 DEG C of normal temperature intensification, keeps 5min; And then 5min to 150 DEG C of intensification, keep 5min; Finally heat up 5min to 180 DEG C, keep 15min.
Hydrochloric acid volumetric concentration in the sample solution that above step (1) constant volume obtains is 30-45%.
In the sample solution that above step (1) constant volume obtains, selenium concentration is controlled within the scope of the concentration gradient of selenium standard solution.
Hydride generation-atomic fluorescence spectrometry described in above step (2) and step (3) is: the reductive agent of employing is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
Above-described solution of potassium borohydride is that potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, is mixed with the solution of potassium borohydride that mass concentration is 8g/L.
The linearly dependent coefficient of the typical curve described in above step (2) requires more than 0.999.
The described radix tetrastigme sample of above step (1) is dried pulverization process in advance, crosses 24 mesh sieves.
Compared to prior art, the present invention has the following advantages and beneficial effect:
1, the present invention adopts micro-wave digestion-hydride generation-AFS DETERMINATION Se content, use Microwave Digestion, avoid the shortcoming that Wet easily pollutes, digestion time is long, do not need to catch up with acid, directly add concentrated hydrochloric acid to carry out the reduction of selenium, simplify and cleared up program, greatly shortened sense cycle.Because of low to the noisy constituent content of selenium in radix tetrastigme, a little less than the interference effect of selenium, do not need to add screener potassium ferricyanide solution, reduce amount of reagent, make step simpler, be easier to operation.
2, the present invention has shortened the cycle that total selenium detects greatly, and originally the shortest sense cycle of method is 8-10 hour, now shortens to 2-3 hour, detects quick, accurate, simple to operate.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
(1) experimental apparatus: the present embodiment atomic fluorescence spectrometer used is the AFS-8220 of Beijing Jitian Instrument Co., Ltd..
(2) sample pre-treatments: radix tetrastigme sample, through cleaning, after 50 DEG C of oven dry, is pulverized with sample grinding machine, crossed 24 mesh sieves, store in valve bag, post label, obtain testing sample, for subsequent use.
(3) reagent and preparation:
Nitric acid (top grade is pure);
Hydrochloric acid (top grade is pure);
Potassium hydroxide (top grade is pure);
Reductive agent: potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, be mixed with the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shakes up, for subsequent use;
Current-carrying: the hydrochloric acid solution that volumetric concentration is 5%
Single element selenium standard solution: 1000mg/L;
The configuration of selenium standard solution: get the selenium national standard solution mother liquor of respective volume, to become concentration be the gradient selenium standard solution of 0-20 μ g/L to stepwise dilution respectively, adds a certain amount of hydrochloric acid before constant volume; Making hydrochloric acid volumetric concentration in selenium standard solution is 30%;
(4) testing sample micro-wave digestion: accurately taking testing sample 0.5g after sieving in micro-wave diminishing pot, add nitric acid 6mL, counteracting tank is placed on electric hot plate, is to clear up half an hour in advance under 100 DEG C of conditions in temperature; Assemble counteracting tank, be placed in microwave dissolver, clear up by the following program of clearing up: power 1600W, 5min to 120 DEG C of normal temperature intensification, keeps 5min; Power 1600W, 5min to 150 DEG C of intensification, keeps 5min; Power 1600W, 5min to 180 DEG C of intensification, keeps 15min DEG C.After having cleared up, add a certain amount of hydrochloric acid, after mixing, allow it slowly be cooled to room temperature, then digestion solution is filtered and is transferred in 25mL volumetric flask, making the volumetric concentration of hydrochloric acid in liquid to be measured is 30%, makes sample solution; Prepare blank sample simultaneously; Sample solution and blank sample all detect with hydride generation-atomic fluorescence spectrometry; The reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
(5) drawing standard curve set up regression equation: get the selenium national standard solution (1000mg/L) of respective volume, stepwise dilution is to 100 μ g/L; Draw respective volume from 100 μ g/L again, be mixed with the selenium standard solution of 0.5 μ g/L, 1.0 μ g/L, 2.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L concentration gradients; Adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, the reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.Metering system: calibration curve method; Reading mode: peak area; Time delay: 1s; Reading duration: 9s.Set after above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first bioassay standard series, drawing standard curve.Carry out again Specimen Determination, measure respectively blank sample and sample solution.With peak area, to selenium mark Huaihe River solution concentration drawing standard curve and set up regression equation, typical curve linearly dependent coefficient is 0.9996.
Be calculated as follows the content of selenium in sample:
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
The preci-sion and accuracy of this method:
National standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tealeaves), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 ginseng) are carried out to the mensuration of Se content, 5 replicate determination values all, in standard value range of uncertainty, the results are shown in Table 1.
Table 1: the measurement result of selenium in standard substance
| Standard substance | Standard value (mg/kg) | Measured value (mean value, n=5) | Standard deviation (%) |
| GSV-2 | 0.12±0.02 | 0.106 | 4.8 |
| GSB-7 | 0.098±0.008 | 0.103 | 3.6 |
| GSB-12 | 0.043±0.015 | 0.038 | 4.5 |
| GSB-18 | 0.012±0.004 | 0.011 | 4.3 |
As can be seen from Table 1, with the measured national standard material of this method, all in the range of uncertainty of standard value, and preci-sion and accuracy is high.
Embodiment 2:
(1) experimental apparatus: the present embodiment atomic fluorescence spectrometer used is the AFS-8220 of Beijing Jitian Instrument Co., Ltd..
(2) sample pre-treatments: radix tetrastigme sample, through cleaning, after 50 DEG C of oven dry, is pulverized with sample grinding machine, crossed 24 mesh sieves, store in valve bag, post label, obtain testing sample, for subsequent use.
(3) reagent and preparation:
Nitric acid (top grade is pure);
Hydrochloric acid (top grade is pure);
Potassium hydroxide (top grade is pure);
Reductive agent: potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, be mixed with the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shakes up, for subsequent use;
Current-carrying: the hydrochloric acid solution that volumetric concentration is 5%
Single element selenium standard solution: 1000mg/L;
The configuration of selenium standard solution: get the selenium national standard solution mother liquor of respective volume, to become concentration be the gradient selenium standard solution of 0-20 μ g/L to stepwise dilution respectively, adds a certain amount of hydrochloric acid before constant volume; Making hydrochloric acid volumetric concentration in selenium standard solution is 35%;
(4) testing sample micro-wave digestion: accurately taking testing sample 0.5g after sieving in micro-wave diminishing pot, add nitric acid 6mL, counteracting tank is placed on electric hot plate, is to clear up half an hour in advance under 100 DEG C of conditions in temperature; Assemble counteracting tank, be placed in microwave dissolver, clear up by the following program of clearing up: power 1600W, 5min to 120 DEG C of normal temperature intensification, keeps 5min; Power 1600W, 5min to 150 DEG C of intensification, keeps 5min; Power 1600W, 5min to 180 DEG C of intensification, keeps 15min DEG C.After having cleared up, add a certain amount of hydrochloric acid, after mixing, allow it slowly be cooled to room temperature, then digestion solution is filtered and is transferred in 25mL volumetric flask, making the volumetric concentration of hydrochloric acid in liquid to be measured is 35%, makes sample solution; Prepare blank sample simultaneously; Sample solution and blank sample all detect with hydride generation-atomic fluorescence spectrometry; The reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
(5) drawing standard curve set up regression equation: get the selenium national standard solution (1000mg/L) of respective volume, stepwise dilution is to 100 μ g/L; Draw respective volume from 100 μ g/L again, be mixed with the selenium standard solution of 0.5 μ g/L, 1.0 μ g/L, 2.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L concentration gradients; Adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, the reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.Metering system: calibration curve method; Reading mode: peak area; Time delay: 1s; Reading duration: 9s.Set after above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first bioassay standard series, drawing standard curve.Carry out again Specimen Determination, measure respectively blank sample and sample solution.With peak area, to selenium mark Huaihe River solution concentration drawing standard curve and set up regression equation, typical curve linearly dependent coefficient is 0.9996.
Be calculated as follows the content of selenium in sample:
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
The preci-sion and accuracy of this method:
National standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tealeaves), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 ginseng) are carried out to the mensuration of Se content, 5 replicate determination values all, in standard value range of uncertainty, the results are shown in Table 2.
The measurement result of selenium in table 2 standard substance
As can be seen from Table 2, with the measured national standard material of this method, all in the range of uncertainty of standard value, and preci-sion and accuracy is high.
Embodiment 3:
(1) experimental apparatus: the present embodiment atomic fluorescence spectrometer used is the AFS-8220 of Beijing Jitian Instrument Co., Ltd..
(2) sample pre-treatments: radix tetrastigme sample, through cleaning, after 55 DEG C of oven dry, is pulverized with sample grinding machine, crossed 24 mesh sieves, store in valve bag, post label, obtain testing sample, for subsequent use.
(3) reagent and preparation:
Nitric acid (top grade is pure);
Hydrochloric acid (top grade is pure);
Potassium hydroxide (top grade is pure);
Reductive agent: potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, be mixed with the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shakes up, for subsequent use;
Current-carrying: the hydrochloric acid solution that volumetric concentration is 5%
Single element selenium standard solution: 1000mg/L;
The configuration of selenium standard solution: get the selenium national standard solution mother liquor of respective volume, to become concentration be the gradient selenium standard solution of 0-20 μ g/L to stepwise dilution respectively, adds a certain amount of hydrochloric acid before constant volume; Making hydrochloric acid volumetric concentration in selenium standard solution is 40%;
(4) testing sample micro-wave digestion: accurately taking testing sample 0.5g after sieving in micro-wave diminishing pot, add nitric acid 6mL, counteracting tank is placed on electric hot plate, is to clear up half an hour in advance under 100 DEG C of conditions in temperature; Assemble counteracting tank, be placed in microwave dissolver, clear up by the following program of clearing up: power 1600W, 5min to 120 DEG C of normal temperature intensification, keeps 5min; Power 1600W, 5min to 150 DEG C of intensification, keeps 5min; Power 1600W, 5min to 180 DEG C of intensification, keeps 15min DEG C.After having cleared up, add a certain amount of hydrochloric acid, after mixing, allow it slowly be cooled to room temperature, then digestion solution is filtered and is transferred in 25mL volumetric flask, making the volumetric concentration of hydrochloric acid in liquid to be measured is 40%, makes sample solution; Prepare blank sample simultaneously; Sample solution and blank sample all detect with hydride generation-atomic fluorescence spectrometry; The reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
(5) drawing standard curve set up regression equation: get the selenium national standard solution (1000mg/L) of respective volume, stepwise dilution is to 100 μ g/L; Draw respective volume from 100 μ g/L again, be mixed with the selenium standard solution of 0.5 μ g/L, 1.0 μ g/L, 2.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L concentration gradients; Adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, the reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.Metering system: calibration curve method; Reading mode: peak area; Time delay: 1s; Reading duration: 9s.Set after above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first bioassay standard series, drawing standard curve.Carry out again Specimen Determination, measure respectively blank sample and sample solution.With peak area, to selenium mark Huaihe River solution concentration drawing standard curve and set up regression equation, typical curve linearly dependent coefficient is 0.9996.
Be calculated as follows the content of selenium in sample:
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
The preci-sion and accuracy of this method:
National standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tealeaves), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 ginseng) are carried out to the mensuration of Se content, 5 replicate determination values all, in standard value range of uncertainty, the results are shown in Table 3.
The measurement result of selenium in table 3 standard substance
Embodiment 4:
(1) experimental apparatus: the present embodiment atomic fluorescence spectrometer used is the AFS-8220 of Beijing Jitian Instrument Co., Ltd..
(2) sample pre-treatments: radix tetrastigme sample, through cleaning, after 55 DEG C of oven dry, is pulverized with sample grinding machine, crossed 24 mesh sieves, store in valve bag, post label, obtain testing sample, for subsequent use.
(3) reagent and preparation:
Nitric acid (top grade is pure);
Hydrochloric acid (top grade is pure);
Potassium hydroxide (top grade is pure);
Reductive agent: potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, be mixed with the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shakes up, for subsequent use;
Current-carrying: the hydrochloric acid solution that volumetric concentration is 5%
Single element selenium standard solution: 1000mg/L;
The configuration of selenium standard solution: get the selenium national standard solution mother liquor of respective volume, to become concentration be the gradient selenium standard solution of 0-20 μ g/L to stepwise dilution respectively, adds a certain amount of hydrochloric acid before constant volume; Making hydrochloric acid volumetric concentration in selenium standard solution is 45%;
(4) testing sample micro-wave digestion: accurately taking testing sample 0.5g after sieving in micro-wave diminishing pot, add nitric acid 6mL, counteracting tank is placed on electric hot plate, is to clear up half an hour in advance under 100 DEG C of conditions in temperature; Assemble counteracting tank, be placed in microwave dissolver, clear up by the following program of clearing up: power 1600W, 5min to 120 DEG C of normal temperature intensification, keeps 5min; Power 1600W, 5min to 150 DEG C of intensification, keeps 5min; Power 1600W, 5min to 180 DEG C of intensification, keeps 15min DEG C.After having cleared up, add a certain amount of hydrochloric acid, after mixing, allow it slowly be cooled to room temperature, then digestion solution is filtered and is transferred in 25mL volumetric flask, making the volumetric concentration of hydrochloric acid in liquid to be measured is 45%, makes sample solution; Prepare blank sample simultaneously; Sample solution and blank sample all detect with hydride generation-atomic fluorescence spectrometry; The reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
(5) drawing standard curve set up regression equation: get the selenium national standard solution (1000mg/L) of respective volume, stepwise dilution is to 100 μ g/L; Draw respective volume from 100 μ g/L again, be mixed with the selenium standard solution of 0.5 μ g/L, 1.0 μ g/L, 2.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L concentration gradients; Adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, the reductive agent that hydride generation-atomic fluorescence spectrometry adopts is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.Metering system: calibration curve method; Reading mode: peak area; Time delay: 1s; Reading duration: 9s.Set after above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first bioassay standard series, drawing standard curve.Carry out again Specimen Determination, measure respectively blank sample and sample solution.With peak area, to selenium mark Huaihe River solution concentration drawing standard curve and set up regression equation, typical curve linearly dependent coefficient is 0.9996.
Be calculated as follows the content of selenium in sample:
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
The preci-sion and accuracy of this method:
National standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tealeaves), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 ginseng) are carried out to the mensuration of Se content, 5 replicate determination values all, in standard value range of uncertainty, the results are shown in Table 4.
The measurement result of selenium in table 4 standard substance
As can be seen from Table 4, with the measured national standard material of this method, all in the range of uncertainty of standard value, and preci-sion and accuracy is high.
Embodiment 5:
GB5009.93-2010 is to same sample measured result difference for comparing embodiment 1 method and national standard " mensuration of national food safety standard selenium in food ".
National standard method detailed rules for the implementation are referring to National Standard of the People's Republic of China's " mensuration of national food safety standard selenium in food " GB5009.93-2010.
Sample detection result is as table 5.
Table 5: radix tetrastigme Selenium In Some Selenium-rich Biological Samples content comparison
| Sample title | This method (mg/kg; N=5) | National standard (mg/kg; N=5) | Relative standard deviation (%) |
| Radix tetrastigme-Zhejiang | 0.102 | 0.105 | -2.9 |
| Radix tetrastigme-Guangxi | 0.046 | 0.050 | -8.3 |
As can be seen from Table 5, the inventive method and national standard Law show no significant difference to the testing result of Se content.
Reference examples:
(1) experimental apparatus: identical with embodiment 1.
(2) sample pre-treatments: identical with embodiment 1.
(3) reagent and preparation: identical with embodiment 1.
(4) testing sample micro-wave digestion: as different from Example 1, carried out catching up with acid treatment, after micro-wave digestion completes, inner canister is cleared up in taking-up, place on electric hot plate and catch up with acid, in the time that digestion solution steams to 1～2mL, add the concentrated hydrochloric acid of 10mL, after mixing, in 100 DEG C of heating 30min, obtain reducing solution, then reducing solution is filtered and is transferred in 25mL volumetric flask, the concentration that makes hydrochloric acid in liquid to be measured is 40%, prepares blank sample simultaneously.Liquid to be measured detects for atomic fluorescence spectrometer.
(5) drawing standard curve set up regression equation: identical with embodiment 1.
The preci-sion and accuracy of this method:
National standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tealeaves), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 ginseng) are carried out to the mensuration of Se content, 5 replicate determination values all, in standard value range of uncertainty, the results are shown in Table 6.
The measurement result of selenium in table 6 standard substance
| Standard substance | Standard value (mg/kg) | Measured value (mean value; N=5) | Standard deviation (%) |
| GSV-2 | 0.12±0.02 | 0.108 | 2.6 |
| GSB-7 | 0.098±0.008 | 0.097 | 2.8 |
| GSB-12 | 0.043±0.015 | 0.039 | 4.3 |
| GSB-18 | 0.012±0.004 | 0.013 | 4.7 |
As can be seen from Table 6, with the measured national standard material of this method, all in the range of uncertainty of standard value, and preci-sion and accuracy is high.
Compared with example 1, though measurement result without impact, this embodiment has carried out catching up with acid treatment, thus digestion time lengthen.
Drawn by above example, Microwave Digestion can greatly shorten digestion time and clear up operation, compares with the content method of national standard Law working sample selenium, greatly shorten digestion time, in situation without screener, substantially unaffected to testing result, reduce the use of reagent.Through catching up with acid and without catching up with acid-treated sample determination result to differ no significant difference, without catching up with acid to shorten the time of clearing up, avoiding the evaporate to dryness because catching up with sour step to bring, contaminated equivalent risk.Method accuracy of the present invention and precision are all very high, and experimental period is short, and operation steps is simple, measure fast.
Claims (8)
1. a method for Se content in Fast Measurement radix tetrastigme, is characterized in that: said method comprising the steps of:
(1) micro-wave digestion: use nitric acid to carry out micro-wave digestion processing to radix tetrastigme sample; Described micro-wave digestion is undertaken by microwave dissolver program, after having cleared up, is that 30-45% hydrochloric acid reduces to radix tetrastigme sample by volumetric concentration, and constant volume obtains sample solution, for subsequent use; Prepare blank sample simultaneously, for subsequent use;
(2) drawing standard curve and set up regression equation: be mixed with the selenium standard solution of concentration gradient as 0-20 μ g/L taking selenium national standard solution as mother liquor, adopt hydride generation-atomic fluorescence spectrometry to measure selenium standard solution, according to the measurement result drawing standard curve of selenium standard solution and set up regression equation;
(3) measure and calculation: blank sample and sample solution are measured by hydride generation-atomic fluorescence spectrometer; Obtain the content of Selenium In Some Selenium-rich Biological Samples according to formula (I):
In formula: the content that X is Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg; C is the concentration that sample solution digestive juice is measured, and unit is μ g/L; C
0for the concentration that blank sample is measured, unit is μ g/L; V is sample constant volume, and unit is mL; M is the sample weighting amount of sample, and unit is a gram g.
2. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 1, is characterized in that: the program of clearing up of the micro-wave digestion described in step (1) is: power is permanent is 1600W, first from 5min to 120 DEG C of normal temperature intensification, keeps 5min; And then 5min to 150 DEG C of intensification, keep 5min; Finally heat up 5min to 180 DEG C, keep 15min.
3. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 1, is characterized in that: the hydrochloric acid volumetric concentration in the sample solution that step (1) constant volume obtains is 30-45%.
4. according to the method for Se content in the arbitrary described a kind of Fast Measurement radix tetrastigme of claim 1 or 3, it is characterized in that: in the sample solution that step (1) constant volume obtains, selenium concentration is controlled within the scope of the concentration gradient of selenium standard solution.
5. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 1, is characterized in that: the hydride generation-atomic fluorescence spectrometry described in step (2) and step (3) is: the reductive agent of employing is potassium borohydride; The condition determination adopting is: negative high voltage is 270V; Lamp current is 80mA; Stove height is 8mm; Flow rate of carrier gas is 300mL/min; Shield gas flow speed is 800mL/min; Current-carrying is that volumetric concentration is 5% hydrochloric acid.
6. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 5, it is characterized in that: described solution of potassium borohydride is that potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, is mixed with the solution of potassium borohydride that mass concentration is 8g/L.
7. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 1, is characterized in that: the linearly dependent coefficient of the typical curve described in step (2) requires more than 0.999.
8. the method for Se content in a kind of Fast Measurement radix tetrastigme according to claim 1, is characterized in that: the described radix tetrastigme sample of step (1) is dried pulverization process in advance, crosses 24 mesh sieves.
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| CN105334094B (en) * | 2015-11-27 | 2018-07-13 | 广西壮族自治区药用植物园 | Detect the pre-treating method of metallic element in common bombax flower Aqueous extracts |
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