CN104122241B - 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, the method for Se content in specifically a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri).
Background technology
Radix Apioris Fortunei (Radix Lespedezae Buergeri) (Tetrastigmatis hemsleyani), also known as：There are angle Herba Cayatiae Japonicae, stone mouse, be that Vitaceae precipice is climbed
Calamus plant, its tuber is referred to as Radix Tetrastigmatis Hemsleyani.Radix Apioris Fortunei (Radix Lespedezae Buergeri) is mainly distributed on the Changjiang river areas to the south, is born in dark and damp hillside, gully or small stream
The other sylvan life of paddy, with tuber or herb people's medicine, is Guangxi conventional Chinese herbal medicine among the people, have antiviral, antiinflammatory, analgesia with antipyretic,
Liver protection etc. acts on, and Small side effects, is " bouvardin " that Western medicine cannot replace.Recent study finds, Radix Apioris Fortunei (Radix Lespedezae Buergeri) acetic acid
Ethyl ester extract is the maximally effective composition of antitumor common drug, and it not only can slow down the growth of cancerous cell, and to hepatocarcinoma and
Blood cell strain has " apoptosis-promoting effect ", and this important discovery has greatly promoted its using value medically and front
Scape.Radix Apioris Fortunei (Radix Lespedezae Buergeri) is used for the Chinese patent medicine production of the types such as antitumor, rheumatism, hepatitis processed, such as Radix Apioris Fortunei (Radix Lespedezae Buergeri) granule, golden stilbene at present
Piece, spun gold ground nail gelatin capsule, Huatuo's rheumatism health-care capsule etc..Clinically it is widely used in anticancer and anti AIDS virus, antitumor, treatment
Hematopathy and cardiovascular and cerebrovascular disease, hepatitis, meningitiss, acute bronchitiss, pneumonia, enteritis and pharyngolaryngitis, infantile hyperpyrexia caused by exogenous pathogenic factor
Etc. disease.
Selenium element is one of trace element needed by human, Keshan disease, Kaschin-Beck disease and the relevant endemic diseases of iodine deficiency, each
Plant cancer, cardiovascular disease, complement activation and epidemic hemorrhagic fever, male infertility and forepart pregnant women hypertension, radiation is damaged
Wound, body reparation and slow down aging, immunologic function and acquired immune deficiency syndrome (AIDS), heavy metal toxicity and occupation disease etc. are all closely related with selenium.Selenium
It is the active center of glutathion peroxidase (GSH-Px).There is anti-cancer, anticancer, antioxidation, prevent multiple endemicity diseases
The effects such as disease, antagonism toxic heavy metal, enhancing body immunity, slow down aging, the liver protecting and cardiac muscle health.
Medicine containing selenium is concentrated mainly on and does hypertension drug, anti-inflammatory drug, cancer therapy drug three broad aspect in the world.Radix Apioris Fortunei (Radix Lespedezae Buergeri)
It is used for cancer therapy drug as a kind of, Se content research is essential.
At present, the assay method of selenium mainly has：Atomic absorption spectrography (AAS), inductively coupled plasma mass spectrometry, ultraviolet are divided
Light photometry, electrochemical methods, Neutron activation analysiss and Hydride Generation-atomic Fluorescence Spectrometry.In these methods,
Hydride Generation-atomic Fluorescence Spectrometry has that detection limit is low, spectral interference is few, chemical interference is low, the range of linearity is wide, operation is simple
Just, the low advantage of operating cost.
The method that hydride generation atomic fluorescence spectrometry disclosed in existing document measures Se content.As《Selenium in feedstuff
Mensure》(GB/T13883-2008)、《The detection method of Folium Camelliae sinensis leaf Se content》(GB/T21729-2008)、《Food safety state
Mensure (GB5009.93-2010) of selenium etc. in family's standard food, said method all adopts Wet, complex operation；Using micro-
When ripple is cleared up, acid treatment need to be caught up with, clear up the cycle long；And in continuous mode, all used hydrochloric acid solution and the ferrum cyanogen of 6mol/L
Change potassium solution, reagent dosage is big, complex operation.
Disclosed had using the method that hydride generation atomic fluorescence spectrometry measures Se content：Number of patent application is
20111027682.0,201110427886.4 and 201110427880.7 Chinese patent application individually disclose quick mensure
The method of plant sample, animal tissue and Selenium in Soils content, all adopts nitric acid-perchloric acid mixed acid Wet, hydrogenation
There is AFS DETERMINATION in thing, but Wet program is loaded down with trivial details, complex operation, and error is big.
The method that presently, there are exist complex operation or the mensure cycle long the shortcomings of.
Content of the invention
In order to overcome the deficiencies in the prior art, the invention provides one kind is simple to operate, accurately quickly measure Radix Apioris Fortunei (Radix Lespedezae Buergeri)
The method of middle Se content.
To achieve these goals, technical scheme is as follows：
In a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri), the method for Se content, comprises the following steps：
(1) micro-wave digestion：Using nitric acid, microwave digestion is carried out to Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample；Described micro-wave digestion presses microwave
Clear up instrument program to carry out, after the completion of clearing up, be that 30-45% hydrochloric acid reduces to Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample with volumetric concentration, constant volume obtains
To sample solution, standby；Prepare blank sample simultaneously, standby；
(2) draw standard curve and set up regression equation：The Concentraton gradient is become to be with selenium national standard solution for mother liquor
The selenium standard solution of 0-20 μ g/L, is measured to selenium standard solution using hydride generation atomic fluorescence spectrometry,
Measurement result according to selenium standard solution is drawn standard curve and is set up regression equation；
(3) measure and calculation：With hydride atomic fluorescence spectrometetry instrument, blank sample and sample solution are measured；
Obtain the content of Selenium In Some Selenium-rich Biological Samples according to public formula I：
In formula：X is the content of Selenium In Some Selenium-rich Biological Samples, and unit is μ g/kg；The concentration that C measures for sample solution Digestive system, unit is
μg/L；C0The concentration measuring for blank sample, unit is μ g/L；V is sample constant volume, and unit is mL；M is the title sample of sample
Amount, unit is gram g.
The program of clearing up of the micro-wave digestion described in above step (1) is：Power is permanent to be 1600W, first from room temperature intensification 5min
To 120 DEG C, keep 5min；Then heat up again 5min to 150 DEG C, keep 5min；Finally intensification 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 controls the Concentraton gradient scope in selenium standard solution
Interior.
Hydride generation atomic fluorescence spectrometry described in above step (2) and step (3) is：Using reduction
Agent is potassium borohydride；Using condition determination be：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Flow rate of carrier gas is
300mL/min；Shield gas flow speed is 800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.
Above-described solution of potassium borohydride is that potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L,
It is configured to the solution of potassium borohydride that mass concentration is 8g/L.
The linearly dependent coefficient of the standard curve described in above step (2) requires more than 0.999.
Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample described in above step (1) carries out dries pulverizing process in advance, crosses 24 mesh sieves.
Compared to prior art, the present invention has advantages below and beneficial effect：
1st, the present invention adopts micro-wave digestion hydride generation atomic fluorescence spectrometry to measure Se content, is disappeared using microwave
Solution, it is to avoid Wet easily pollutes, the shortcoming of digestion time length, is not required to catch up with acid, be directly added into concentrated hydrochloric acid carry out selenium also
Former, simplify and clear up program, greatly shorten detection cycle.Because low to the noisy constituent content of selenium in Radix Apioris Fortunei (Radix Lespedezae Buergeri), selenium is done
The effect of disturbing is weak, is not required to add screener potassium ferricyanide solution, decreases amount of reagent, makes step simpler it is easier to operate.
2nd, the present invention substantially reduces the cycle of total selenium detection, and the originally the shortest detection cycle of method is 8-10 hour, existing
Shorten to 2-3 hour, detection is quick, accurate, simple to operate.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1：
(1) experimental apparatus：Atomic fluorescence spectrometer used by the present embodiment is Beijing Jitian Instrument Co., Ltd. AFS-
8220.
(2) sample pre-treatments：By Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample through cleaning, after 50 DEG C dry, pulverized with sample grinding machine, cross 24 mesh sieves, storage
In valve bag, post label, obtain testing sample, standby.
(3) reagent and preparation：
Nitric acid (top pure grade)；
Hydrochloric acid (top pure grade)；
Potassium hydroxide (top pure grade)；
Reducing agent：Potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, prepares
Become the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shake up, standby；
Current-carrying：Volumetric concentration is 5% hydrochloric acid solution
Single element selenium standard solution：1000mg/L；
The configuration of selenium standard solution：Take the selenium national standard solution mother solution of respective volume, stepwise dilution becomes concentration respectively
Gradient selenium standard solution for 0-20 μ g/L, adds a certain amount of hydrochloric acid before constant volume；Make hydrochloric acid volume in selenium standard solution
Concentration is 30%；
(4) testing sample micro-wave digestion：Accurately weigh the testing sample 0.5g after sieving in micro-wave diminishing pot, add nitre
Sour 6mL, counteracting tank is placed on electric hot plate, clears up half an hour in advance under the conditions of temperature is 100 DEG C；Assemble counteracting tank, put
In microwave dissolver, cleared up by following program of clearing up：Power 1600W, intensification 5min to 120 DEG C of room temperature, keep 5min；
Power 1600W, keeps 5min by intensification 5min to 150 DEG C；Power 1600W, keeps 15min DEG C by intensification 5min to 180 DEG C.Clear up
After the completion of, add a certain amount of hydrochloric acid, after mixing, allow it be slowly cooled to room temperature, then digestion solution filtration is transferred to 25mL and hold
In measuring bottle, the volumetric concentration making hydrochloric acid in prepare liquid is 30%, makes sample solution；Prepare blank sample simultaneously；Sample solution
All detected with hydride generation atomic fluorescence spectrometry with blank sample；Hydride generation atomic fluorescence spectrometry adopts
Reducing agent is potassium borohydride；Using condition determination be：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Carrier gas stream
Speed is 300mL/min；Shield gas flow speed is 800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.
(5) draw standard curve and set up regression equation：Take selenium national standard solution (1000mg/L) of respective volume, by
Level is diluted to 100 μ g/L；Draw respective volume from 100 μ g/L again, be configured to 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, the selenium standard solution of 20.0 μ g/L Concentraton gradient；Using hydride generation atomic fluorescence spectrometry to selenium
Standard solution is measured, and the reducing agent that hydride generation atomic fluorescence spectrometry adopts is potassium borohydride；Using survey
Fixed condition is：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Flow rate of carrier gas is 300mL/min；Shield gas flow speed is
800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.Metering system：Standard curve method；Reading mode：Peak area；Postpone
Time：1s；Reading duration：9s.After setting above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first
Bioassay standard series, draws standard curve.Carry out Specimen Determination again, measure blank sample and sample solution respectively.With peak area
Standard curve is drawn to selenium mark Huaihe River solution concentration and sets up regression equation, standard curve linearly dependent coefficient is 0.9996.
It is calculated as follows the content of selenium in sample：
In formula：X is the content of Selenium In Some Selenium-rich Biological Samples, and unit is μ g/kg；The concentration that C measures for sample solution Digestive system, unit is
μg/L；C0The concentration measuring for blank sample, unit is μ g/L；V is sample constant volume, and unit is mL；M is the title sample of sample
Amount, unit is gram g.
The preci-sion and accuracy of this method：
To national standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tea
Leaf), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 Radix Ginseng) carry out the mensure of Se content, 5 times parallel assay value is equal
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 (meansigma methodss, 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 national standard material measured by this method all in the range of uncertainty of standard value,
And preci-sion and accuracy is high.
Embodiment 2：
(1) experimental apparatus：Atomic fluorescence spectrometer used by the present embodiment is Beijing Jitian Instrument Co., Ltd. AFS-
8220.
(2) sample pre-treatments：By Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample through cleaning, after 50 DEG C dry, pulverized with sample grinding machine, cross 24 mesh sieves, storage
In valve bag, post label, obtain testing sample, standby.
(3) reagent and preparation：
Nitric acid (top pure grade)；
Hydrochloric acid (top pure grade)；
Potassium hydroxide (top pure grade)；
Reducing agent：Potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, prepares
Become the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shake up, standby；
Current-carrying：Volumetric concentration is 5% hydrochloric acid solution
Single element selenium standard solution：1000mg/L；
The configuration of selenium standard solution：Take the selenium national standard solution mother solution of respective volume, stepwise dilution becomes concentration respectively
Gradient selenium standard solution for 0-20 μ g/L, adds a certain amount of hydrochloric acid before constant volume；Make hydrochloric acid volume in selenium standard solution
Concentration is 35%；
(4) testing sample micro-wave digestion：Accurately weigh the testing sample 0.5g after sieving in micro-wave diminishing pot, add nitre
Sour 6mL, counteracting tank is placed on electric hot plate, clears up half an hour in advance under the conditions of temperature is 100 DEG C；Assemble counteracting tank, put
In microwave dissolver, cleared up by following program of clearing up：Power 1600W, intensification 5min to 120 DEG C of room temperature, keep 5min；
Power 1600W, keeps 5min by intensification 5min to 150 DEG C；Power 1600W, keeps 15min DEG C by intensification 5min to 180 DEG C.Clear up
After the completion of, add a certain amount of hydrochloric acid, after mixing, allow it be slowly cooled to room temperature, then digestion solution filtration is transferred to 25mL and hold
In measuring bottle, the volumetric concentration making hydrochloric acid in prepare liquid is 35%, makes sample solution；Prepare blank sample simultaneously；Sample solution
All detected with hydride generation atomic fluorescence spectrometry with blank sample；Hydride generation atomic fluorescence spectrometry adopts
Reducing agent is potassium borohydride；Using condition determination be：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Carrier gas stream
Speed is 300mL/min；Shield gas flow speed is 800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.
(5) draw standard curve and set up regression equation：Take selenium national standard solution (1000mg/L) of respective volume, by
Level is diluted to 100 μ g/L；Draw respective volume from 100 μ g/L again, be configured to 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, the selenium standard solution of 20.0 μ g/L Concentraton gradient；Using hydride generation atomic fluorescence spectrometry to selenium
Standard solution is measured, and the reducing agent that hydride generation atomic fluorescence spectrometry adopts is potassium borohydride；Using survey
Fixed condition is：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Flow rate of carrier gas is 300mL/min；Shield gas flow speed is
800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.Metering system：Standard curve method；Reading mode：Peak area；Postpone
Time：1s；Reading duration：9s.After setting above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first
Bioassay standard series, draws standard curve.Carry out Specimen Determination again, measure blank sample and sample solution respectively.With peak area
Standard curve is drawn to selenium mark Huaihe River solution concentration and sets up regression equation, standard curve linearly dependent coefficient is 0.9996.
It is calculated as follows the content of selenium in sample：
In formula：X is the content of Selenium In Some Selenium-rich Biological Samples, and unit is μ g/kg；The concentration that C measures for sample solution Digestive system, unit is
μg/L；C0The concentration measuring for blank sample, unit is μ g/L；V is sample constant volume, and unit is mL；M is the title sample of sample
Amount, unit is gram g.
The preci-sion and accuracy of this method：
To national standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tea
Leaf), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 Radix Ginseng) carry out the mensure of Se content, 5 times parallel assay value is equal
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 national standard material measured by this method all in the range of uncertainty of standard value,
And preci-sion and accuracy is high.
Embodiment 3：
(1) experimental apparatus：Atomic fluorescence spectrometer used by the present embodiment is Beijing Jitian Instrument Co., Ltd. AFS-
8220.
(2) sample pre-treatments：By Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample through cleaning, after 55 DEG C dry, pulverized with sample grinding machine, cross 24 mesh sieves, storage
In valve bag, post label, obtain testing sample, standby.
(3) reagent and preparation：
Nitric acid (top pure grade)；
Hydrochloric acid (top pure grade)；
Potassium hydroxide (top pure grade)；
Reducing agent：Potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, prepares
Become the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shake up, standby；
Current-carrying：Volumetric concentration is 5% hydrochloric acid solution
Single element selenium standard solution：1000mg/L；
The configuration of selenium standard solution：Take the selenium national standard solution mother solution of respective volume, stepwise dilution becomes concentration respectively
Gradient selenium standard solution for 0-20 μ g/L, adds a certain amount of hydrochloric acid before constant volume；Make hydrochloric acid volume in selenium standard solution
Concentration is 40%；
(4) testing sample micro-wave digestion：Accurately weigh the testing sample 0.5g after sieving in micro-wave diminishing pot, add nitre
Sour 6mL, counteracting tank is placed on electric hot plate, clears up half an hour in advance under the conditions of temperature is 100 DEG C；Assemble counteracting tank, put
In microwave dissolver, cleared up by following program of clearing up：Power 1600W, intensification 5min to 120 DEG C of room temperature, keep 5min；
Power 1600W, keeps 5min by intensification 5min to 150 DEG C；Power 1600W, keeps 15min DEG C by intensification 5min to 180 DEG C.Clear up
After the completion of, add a certain amount of hydrochloric acid, after mixing, allow it be slowly cooled to room temperature, then digestion solution filtration is transferred to 25mL and hold
In measuring bottle, the volumetric concentration making hydrochloric acid in prepare liquid is 40%, makes sample solution；Prepare blank sample simultaneously；Sample solution
All detected with hydride generation atomic fluorescence spectrometry with blank sample；Hydride generation atomic fluorescence spectrometry adopts
Reducing agent is potassium borohydride；Using condition determination be：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Carrier gas stream
Speed is 300mL/min；Shield gas flow speed is 800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.
(5) draw standard curve and set up regression equation：Take selenium national standard solution (1000mg/L) of respective volume, by
Level is diluted to 100 μ g/L；Draw respective volume from 100 μ g/L again, be configured to 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, the selenium standard solution of 20.0 μ g/L Concentraton gradient；Using hydride generation atomic fluorescence spectrometry to selenium
Standard solution is measured, and the reducing agent that hydride generation atomic fluorescence spectrometry adopts is potassium borohydride；Using survey
Fixed condition is：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Flow rate of carrier gas is 300mL/min；Shield gas flow speed is
800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.Metering system：Standard curve method；Reading mode：Peak area；Postpone
Time：1s；Reading duration：9s.After setting above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first
Bioassay standard series, draws standard curve.Carry out Specimen Determination again, measure blank sample and sample solution respectively.With peak area
Standard curve is drawn to selenium mark Huaihe River solution concentration and sets up regression equation, standard curve linearly dependent coefficient is 0.9996.
It is calculated as follows the content of selenium in sample：
In formula：X is the content of Selenium In Some Selenium-rich Biological Samples, and unit is μ g/kg；The concentration that C measures for sample solution Digestive system, unit is
μg/L；C0The concentration measuring for blank sample, unit is μ g/L；V is sample constant volume, and unit is mL；M is the title sample of sample
Amount, unit is gram g.
The preci-sion and accuracy of this method：
To national standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tea
Leaf), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 Radix Ginseng) carry out the mensure of Se content, 5 times parallel assay value is equal
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：Atomic fluorescence spectrometer used by the present embodiment is Beijing Jitian Instrument Co., Ltd. AFS-
8220.
(2) sample pre-treatments：By Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample through cleaning, after 55 DEG C dry, pulverized with sample grinding machine, cross 24 mesh sieves, storage
In valve bag, post label, obtain testing sample, standby.
(3) reagent and preparation：
Nitric acid (top pure grade)；
Hydrochloric acid (top pure grade)；
Potassium hydroxide (top pure grade)；
Reducing agent：Potassium borohydride, appropriate potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5g/L, prepares
Become the solution of potassium borohydride that mass concentration is 8g/L, constant volume, shake up, standby；
Current-carrying：Volumetric concentration is 5% hydrochloric acid solution
Single element selenium standard solution：1000mg/L；
The configuration of selenium standard solution：Take the selenium national standard solution mother solution of respective volume, stepwise dilution becomes concentration respectively
Gradient selenium standard solution for 0-20 μ g/L, adds a certain amount of hydrochloric acid before constant volume；Make hydrochloric acid volume in selenium standard solution
Concentration is 45%；
(4) testing sample micro-wave digestion：Accurately weigh the testing sample 0.5g after sieving in micro-wave diminishing pot, add nitre
Sour 6mL, counteracting tank is placed on electric hot plate, clears up half an hour in advance under the conditions of temperature is 100 DEG C；Assemble counteracting tank, put
In microwave dissolver, cleared up by following program of clearing up：Power 1600W, intensification 5min to 120 DEG C of room temperature, keep 5min；
Power 1600W, keeps 5min by intensification 5min to 150 DEG C；Power 1600W, keeps 15min DEG C by intensification 5min to 180 DEG C.Clear up
After the completion of, add a certain amount of hydrochloric acid, after mixing, allow it be slowly cooled to room temperature, then digestion solution filtration is transferred to 25mL and hold
In measuring bottle, the volumetric concentration making hydrochloric acid in prepare liquid is 45%, makes sample solution；Prepare blank sample simultaneously；Sample solution
All detected with hydride generation atomic fluorescence spectrometry with blank sample；Hydride generation atomic fluorescence spectrometry adopts
Reducing agent is potassium borohydride；Using condition determination be：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Carrier gas stream
Speed is 300mL/min；Shield gas flow speed is 800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.
(5) draw standard curve and set up regression equation：Take selenium national standard solution (1000mg/L) of respective volume, by
Level is diluted to 100 μ g/L；Draw respective volume from 100 μ g/L again, be configured to 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, the selenium standard solution of 20.0 μ g/L Concentraton gradient；Using hydride generation atomic fluorescence spectrometry to selenium
Standard solution is measured, and the reducing agent that hydride generation atomic fluorescence spectrometry adopts is potassium borohydride；Using survey
Fixed condition is：Negative high voltage is 270V；Lamp current is 80mA；The a height of 8mm of stove；Flow rate of carrier gas is 300mL/min；Shield gas flow speed is
800mL/min；The hydrochloric acid that current-carrying is 5% for volumetric concentration.Metering system：Standard curve method；Reading mode：Peak area；Postpone
Time：1s；Reading duration：9s.After setting above-mentioned parameter, combustion preheater 10-20min starts to measure after instrument stabilizer, first
Bioassay standard series, draws standard curve.Carry out Specimen Determination again, measure blank sample and sample solution respectively.With peak area
Standard curve is drawn to selenium mark Huaihe River solution concentration and sets up regression equation, standard curve linearly dependent coefficient is 0.9996.
It is calculated as follows the content of selenium in sample：
In formula：X is the content of Selenium In Some Selenium-rich Biological Samples, and unit is μ g/kg；The concentration that C measures for sample solution Digestive system, unit is
μg/L；C0The concentration measuring for blank sample, unit is μ g/L；V is sample constant volume, and unit is mL；M is the title sample of sample
Amount, unit is gram g.
The preci-sion and accuracy of this method：
To national standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tea
Leaf), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 Radix Ginseng) carry out the mensure of Se content, 5 times parallel assay value is equal
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 national standard material measured by this method all in the range of uncertainty of standard value,
And preci-sion and accuracy is high.
Embodiment 5：
Comparing embodiment 1 method and national standard《The mensure of national food safety standard selenium in food》GB5009.93-
2010 pairs of same sample measured result differences.
National standard method detailed rules for the implementation are referring to National Standard of the People's Republic of China《National food safety standard selenium in food
Measure》GB5009.93-2010.
Sample detection result such as table 5.
Table 5：Radix Apioris Fortunei (Radix Lespedezae Buergeri) Selenium In Some Selenium-rich Biological Samples comparision contents
| Sample ID | This method (mg/kg；N=5) | National standard (mg/kg；N=5) | Relative standard deviation (%) |
| Radix Apioris Fortunei (Radix Lespedezae Buergeri) Zhejiang | 0.102 | 0.105 | -2.9 |
| Radix Apioris Fortunei (Radix Lespedezae Buergeri) 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：Same as Example 1.
(2) sample pre-treatments：Same as Example 1.
(3) reagent and preparation：Same as Example 1.
(4) testing sample micro-wave digestion：As different from Example 1, carried out catching up with acid treatment, that is, micro-wave digestion completes
Afterwards, take out and clear up inner canister, place and carry out catching up with acid on electric hot plate, when digestion solution steams to 1～2mL, add the concentrated hydrochloric acid of 10mL, mix
After even, heat 30min in 100 DEG C, obtain reducing solution, then reducing solution filtration is transferred in 25mL volumetric flask, make in prepare liquid
The concentration of hydrochloric acid is 40%, prepares blank sample simultaneously.Prepare liquid is used for atomic fluorescence spectrometer and detects.
(5) draw standard curve and set up regression equation：Same as Example 1.
The preci-sion and accuracy of this method：
To national standard material GBW07603 (GSV-2 biochemical component standard substance), GBW10016 (GSB-7 tea
Leaf), GBW10021 (GSB-12 fresh kidney beans), GBW10027 (GSB-18 Radix Ginseng) carry out the mensure of Se content, 5 times parallel assay value is equal
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 (meansigma methodss；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 national standard material measured by 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 no affects, this embodiment has carried out catching up with acid treatment, so digestion time adds
Long.
Drawn by above example, Microwave Digestion is substantially shorter digestion time and clears up operation, and national standard Law is surveyed
The content method of random sample product selenium is compared, and substantially reduces digestion time, in the case of screener, to testing result substantially not
Impacted, reduce the use of reagent.Through catching up with acid to differ no significant difference with without the sample determination result catching up with acid treatment, without catching up with
Time of clearing up is shortened in acid, it is to avoid because catch up with that sour step may bring be evaporated, contaminated equivalent risk.Method of the present invention accuracy
All very high with precision, and experimental period is short, and operating procedure is simple, measures quick.
Claims (5)
1. in a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri) Se content method it is characterised in that：The method comprising the steps of：
（1）Micro-wave digestion：Using nitric acid, microwave digestion is carried out to Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample；Described micro-wave digestion presses micro-wave digestion
Instrument program is carried out, and after the completion of clearing up, is that 30-45% hydrochloric acid reduces to Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample with volumetric concentration, constant volume obtains sample
Solution, standby, the hydrochloric acid volumetric concentration in the sample solution obtaining is 30-45%；Prepare blank sample simultaneously, standby；
（2）Draw standard curve and set up regression equation：Concentraton gradient is become as 0-20 for mother liquor with selenium national standard solution
The selenium standard solution of μ g/L, is measured to selenium standard solution using hydride generation atomic fluorescence spectrometry, according to
The measurement result of selenium standard solution is drawn standard curve and is set up regression equation；
（3）Measure and calculation：With hydride atomic fluorescence spectrometetry instrument, blank sample and sample solution are measured；According to
Formula（Ⅰ）Obtain the content of Selenium In Some Selenium-rich Biological Samples：
X=（C-C 0 ）×V/m（Ⅰ）
In formula：XFor the content of Selenium In Some Selenium-rich Biological Samples, unit is μ g/kg；CThe concentration measuring for sample solution Digestive system, unit is μ g/
L；C 0 The concentration measuring for blank sample, unit is μ g/L；VFor sample constant volume, unit is mL；mFor the sample weighting amount of sample,
Unit is gram g；
Using reducing agent be solution of potassium borohydride；Using condition determination be：Negative high voltage is 270 V；Lamp current is 80 mA；
A height of 8 mm of stove；Flow rate of carrier gas is 300 mL/min；Shield gas flow speed is 800 mL/min；Current-carrying is 5 % for volumetric concentration
Hydrochloric acid；Described solution of potassium borohydride is that potassium borohydride is dissolved in the potassium hydroxide solution that mass concentration is 5 g/L, is configured to
Mass concentration is the solution of potassium borohydride of 8 g/L.
2. in a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri) according to claim 1 Se content method it is characterised in that：Step（1）
The program of clearing up of described micro-wave digestion is：Power is permanent to be 1600 W, first heats up 5 min to 120 DEG C from room temperature, keeps 5
min；Then heat up again 5 min to 150 DEG C, keep 5 min；Finally heat up 5 min to 180 DEG C, keep 15 min.
3. in a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri) according to claim 1 Se content method it is characterised in that：Step（1）
In the sample solution that constant volume obtains, selenium concentration controls in the range of the Concentraton gradient of selenium standard solution.
4. in a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri) according to claim 1 Se content method it is characterised in that：Step（2）
The linearly dependent coefficient of described standard curve requires more than 0.999.
5. in a kind of quick mensure Radix Apioris Fortunei (Radix Lespedezae Buergeri) according to claim 1 Se content method it is characterised in that：Step（1）
Described Radix Apioris Fortunei (Radix Lespedezae Buergeri) sample carries out dries pulverizing process in advance, crosses 24 mesh sieves.
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