CN1200278C - Method of decomposing food sample using micro wave - Google Patents
Method of decomposing food sample using micro wave Download PDFInfo
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- CN1200278C CN1200278C CN 03112142 CN03112142A CN1200278C CN 1200278 C CN1200278 C CN 1200278C CN 03112142 CN03112142 CN 03112142 CN 03112142 A CN03112142 A CN 03112142A CN 1200278 C CN1200278 C CN 1200278C
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The present invention relates to a method for decomposing food samples by using microwaves, which belongs to the technical field of physical and chemical inspection for food sanitation. The present invention comprises: a microwave decomposing instrument is used and a nitric acid-hydrogen peroxide or nitric acid and solid, or semi-solid or vegetable oil food sample is quantitatively put into a decomposing pot; 0.5 to 1.2 ml of pure aqua fortis is added and is placed for 10 to 15 min; 0 to 0.5 ml of 30% hydrogen peroxide is added and is placed for 10 to 15 min, and water is added to 8 to 15 ml; the sample is lightly shaken up and a decomposing device is properly installed and is put into the microwave decomposing instrument for decomposing at temperature from 100 to 185 DEG C, and automatic cooling is carried out after finishing the reaction. The method of the present invention has the advantages of a small quantity of reagents, low blank values and accurate measured results, and avoids environmental pollution and experimenters' physical harmfulness caused by a traditional decomposing method. Sample solution decomposed in the method can be used for measuring various microelements, macro-elements and rare-earth elements in food.
Description
(1) method field
The present invention relates to a kind of method, belong to food hygiene physical and chemical inspection technical field, be specifically related to clear up the sample technical field with the micro-wave digestion food samples.
(2) background method
1975, American scholar K.E Jia Weisi waited to propose first to clear up sample with microwave technology, saw to be stated from " inductivity coupled plasma mass spectrometry handbook Atomic Energy Press, 1997:140-151.In recent years, the report of relevant microwave sampling technology was more, as Li Ming etc., and the application of microwave high pressure digestion method in sample decomposes, physical and chemical inspection (chemical handbook), 1988,24 (5); Dai Jingjing etc., inductive coupling plasma mass method is measured the method research of metallic element in the tealeaves, Chinese public health, 2002,18 (10): 1246; Xie Jianbin etc., micro-wave digestion/ICP-MS method is measured human body lung and kidney middle rare earth element, Chinese public health 2002,18 (12): 1502-1504.But prior art nitric acid-hydrogen peroxide use amount in digestion process all requires to use the 6-8ml red fuming nitric acid (RFNA) than the method for big and microwave dissolver manufacturer initial recommendations, these methods generate, and to clear up thing acidity very strong, when surveying arsenic, lead with atomic fluorescence, because of generating white suspension thing and precipitation, and there is bubble to produce frequently, and influence measurement result, during with elements such as graphite furnace sounding lead, cadmium, chromium, because the acid amount is excessive, influence the life-span of graphite-pipe, acidity is strong excessively simultaneously, and most of instrument is all had very strong corrosivity.
" food hygienic standard service manual physical and chemical inspection method " (GB/T5009-1996) in, in sample preparation, have the Microwave Digestion the lead in the food, total mercury, cadmium, chromium, also do not do regulation in the working sample disposal route to other elements, usually will be with 2-4 kind digestion procedure to the analysis of multiple metallic element in the sample, so, increased workload greatly, reduced work efficiency, business efficiency significantly reduces.
(3) summary of the invention
The present invention is directed to the deficiency of food samples disposal route in the prior art and the defective of original micro-wave digestion method, a kind of method of micro-wave digestion food samples is provided, nitric acid-hydrogen peroxide, nitric acid use amount have been reduced widely, reduce treatment step, increase work efficiency, measurement result accurately and reliably.
The inventive method comprises uses microwave dissolver and nitric acid-hydrogen peroxide or nitric acid, and concrete operations are:
(1) digestion solution prepares, and takes by weighing the even food samples 0.2～1.0g of solid, semisolid or vegetable oil, and imbitition sample 0.5～3.0ml places counteracting tank, and alcoholic sample discharges water earlier to bathe and removes alcohol, adds the pure red fuming nitric acid (RFNA) (ρ of top grade
20=1.42g/ml) 0.5～1.0ml places 10～15min; Add pure 30% hydrogen peroxidase 10 of top grade～0.5ml, place 10～15min, add water to 8～15ml;
(2) above-mentioned sample is shaken up gently, adorn appropriate digestion instrument, and put it in the microwave dissolver, clear up, temperature 100-185 ℃, reaction finishes back cooling automatically.
Take out counteracting tank, sample is settled to 15～25ml, be used for measuring.
Measure elements such as iron, manganese, copper, zinc, calcium, magnesium, lead, cadmium, chromium, mercury, arsenic with atomic absorption spectrophotometer (AAS), atomic fluorescence spectrophotometer and inductive coupling plasma emission spectrometer.
When above-mentioned digestion solution prepared, the solid food amount of samples was 0.2～1.0g; Vegetable oil amount of samples 0.2～0.43g.
When above-mentioned digestion solution prepares,, during with acid amount＜1.0ml, can not add hydrogen peroxide for the sample of easily clearing up.
When above-mentioned digestion solution prepared, salted vegetables, vegetables or fruit sample added red fuming nitric acid (RFNA) 0.5～1.0ml, 30% hydrogen peroxidase 10 .0～0.3ml.
When above-mentioned digestion solution prepared, fruit juice, vinegar, soy sauce, milk-contained drink or various wine sample added red fuming nitric acid (RFNA) 0.7～1.0ml, 30% hydrogen peroxidase 10 .0～0.3ml.
When above-mentioned digestion solution prepares, add red fuming nitric acid (RFNA) 0.8～1.0ml for fatty few cake, wheaten food, candy, honey, milk, marine product or each wrapping paper sample, 30% hydrogen peroxidase 10 .3～0.5ml;
When above-mentioned digestion solution prepares, add red fuming nitric acid (RFNA) 1.0ml, 30% hydrogen peroxidase 10 .5ml for ice cream, ice cream, tealeaves, solid health food, milk powder, bean powder, coffee, meat, fat cake, peanut oil or soya-bean oil sample.
Above-mentioned micro-wave digestion can divide 2-3 step to finish, and temperature, pressure progressively raise, in each step, be warmed up in the climbing time of 3～8min fixed temperature.
Clear up program and clear up that the result is auspicious to see Table 1
Table 1 is cleared up program and is cleared up the result
Sample type sample size HNO
3+ H
2O
2Step climbing temperature, pressure keeps clearing up
(g/ml) (ml) rapid (min) (℃) (psi) (min) effect
Cake (fatty clarification, saturating
Few) wheaten food, sugared 0.5 1.0+0.5 15 110 80 5 be bright, pale yellow
Really, honey, sea 25 175 300 15 looks
Product, lime-preserved egg
Ice cream, ice swash
Icepro, tealeaves, guarantor 0.5 1.0+0.5 15 110 100 5 clarifications, saturating
Strong product, milk powder, 25 175 400 20 bright, pale yellow
Bean powder, coffee, look
Meat, cake
(fat)
Peanut oil, soya-bean oil 0.3 1.0+0.5 15 110 100 5 clarifications, saturating
25 185 400 20 is bright, pale yellow
Look
Salted vegetables, concentrated fruit 0.5 0.5+0.2 13 105 50 3 clarifications, saturating
Juice, fruit, vegetables 25 185 250 15 are bright, colourless
Dish
Fruit syrup, vinegar, 0.5 0.7+0.3,13 105 50 3 clarifications, saturating
Soy sauce, to contain breast drink 24 170 270 15 bright, colourless
Material
0.5 1.0+0.3 14 110 80 4 is clear, saturating for the varieties of food items bag
Dress paper, milk 25 175 300 20 is bright, colourless
The accuracy experiment of inventive method:
Find that by check and analysis GBW08508 ground rice and GBW08505 tealeaves the method is all very high to the recovery of iron, manganese, copper, zinc, lead, cadmium, mercury, arsenic, measured value and standard value match, the accuracy and the precision that show method are good, the measurement result of some element sees Table 2 in the GBW08505 tealeaves, and the measurement result of some element sees Table 3 in the GBW08508 ground rice.
The measurement result of some element in the table 2 GBW08505 tealeaves
The element standard value measured value relative standard deviation recovery
(mg/Kg) (mg/Kg) (％) (％)
Fe 373±23 358 1.0 96.0
Mn 766±28 750 0.6 97.9
Cu 16.2±1.9 16.5 0.4 101.8
Zn 38.7±3.9 39.7 1.2 102.6
Pb 1.06±0.10 1.01 3.2 95.3
Cd 0.032±0.005 0.034 4.5 106.2
As 0.191±0.027 0.188 5.2 98.4
The measurement result of some element in the table 3 GBW08508 ground rice
The element standard value measured value relative standard deviation recovery
(mg/Kg) (mg/Kg) (％) (％)
Fe 43.2±3.0 43.05 0.98 99.6
Mn 28.4±3.8 27.21 0.45 95.8
Cu 3.6±0.4 3.64 0.33 101.1
Zn 18.0±1.0 18.46 1.1 102.6
Hg 0.038±0.005 0.037 4.3 97.4
Method of the present invention is used for measuring elements such as the iron, manganese, copper, zinc, lead, cadmium, arsenic, mercury, chromium, nickel, tin, selenium, calcium, potassium, sodium, magnesium, phosphorus, sulphur, molybdenum, vanadium of food.
The characteristics of the inventive method:
1. use amount of reagent few with relevant bibliographical information consumption than instrument manufacturer recommend method, blank value reduces, and has avoided because of adding the interference that the acid amount is brought greatly.
2. digestion solution need not to catch up with acid, can be directly used in the mensuration of atomic absorption spectrophotometer (AAS), atomic fluorescence spectrophotometer and inductive coupling plasma emission spectrograph, avoided because of catching up with the loss or the pollution of the element to be measured that acid causes, simplified operation steps simultaneously, shorten the working time, improved work efficiency.
3. clear up satisfactory for resultly, digestion solution is clear, and the Specimen eliminating liquid that has is for yellow, but measurement result is had no effect.
4. security is big, with the same sample of equal in quality, clears up same clearing up under the program, and the pressure ratio that this law produced adds about the low 50psi of method of 6ml nitric acid.
5. because of using amount of reagent significantly to reduce, reduced nitric acid and decomposed the oxides of nitrogen that produces to the pollution of environment with to experimenter's health harm, economic benefit and ecological benefits obviously improve.
(4) embodiment
Embodiment 1.
1. instrument and reagent: MARS5 microwave dissolver (U.S. CE M company), AA-6800 type atomic absorption spectrophotometer (AAS) (day island proper Tianjin company), AF-610A atomic fluorescence spectrophotometer (second optical instrument factory, Beijing), AE-240 full-automatic electronic balance (Switzerland), to IV computer processing system and hp1000 printer, iron, manganese, copper, zinc, lead, cadmium, arsenic, mercury hollow cathode lamp.Pure nitric acid (the ρ of top grade
20=1.42g/ml), pure 30% hydrogen peroxide of top grade, the metal standard solution is ρ (B)=1mg/ml (State Standard Matter Research Centre), iron, manganese, copper, zinc, lead, cadmium standard use liquid to face with preceding nitric acid stepwise dilution with 0.5mol/L, the mercury standard uses liquid to face with the preceding 1+9 of using nitric acid stepwise dilution, and the arsenic standard uses liquid to face with preceding water stepwise dilution potassium borohydride 0.1g/L (survey mercury), potassium borohydride 10g/L (survey arsenic), thiocarbamide 50g/L.
2. Specimen eliminating: precision takes by weighing pulverizes mixing sample tealeaves (one-level Xihu Longjing Tea) 0.5 gram, place the teflon counteracting tank, add nitric acid 1.0ml, place 15min, add hydrogen peroxidase 10 .5ml and soak 15min, add water to 8ml, shake gently, adorn appropriate digestion instrument, connect temperature, pressure probe, and put it in the microwave dissolver, to select to clear up program according to table 1, power is pressed 1-3 sample 300W, 4-6 sample 600W, 7-12 sample 1200W clears up, and reaction finishes back cooling automatically.During the pressure of indication in the container＜50psi, slowly open, discharge surplus pressure, take out temperature, pressure probe, open each jar successively, sample is settled to 15ml from blow-out disc.
3. assay method: iron, manganese, copper, zinc are measured with flame atomic absorption spectrophotometer, use air-acetylene flame, and instrument slit, air and acetylene flow, lamp holder height, element lamp electric current etc. all transfer to optimum condition by the instrument explanation; With sampling Graphite Furnace Atomic Absorption spectrophotometric determination lead, cadmium, ashing temperature lead is 500 ℃, and cadmium is 500 ℃, atomization temperature lead is 1700 ℃, and cadmium is 1650 ℃, at first enters blank value and measures state, mark is accurate serial then, and sequentially determining is cleared up blank again, sample solution.Arsenic, mercury select for use atomic fluorescence spectrophotometer to measure, and negative high voltage arsenic is 260V, and mercury is 240V, lamp current arsenic is 60mA, and mercury is 40mA, carrier gas flux arsenic 800mL/min, mercury is 600mL/min, and potassium borohydride arsenic is 10g/L, and mercury is that 0.1g/L clears up blank, sample solution with the calibration curve method sequentially determining.
4. measurement result: see Table 4.
The measurement result of element (mg/Kg) in table 4 sample
Sample title Fe Mn Cu Zn Pb Cd As Hg
One-level Longjing tea 149.06 621.63 20.40 45.45 0.32 0.040 0.143 0.019
Soy meal 64.65 19.42 5.15 18.65 0.17 0.093 0.175-
Embodiment 2. is as described in the embodiment 1, and different is that food samples is a soy meal, and measurement result sees Table 4.
Embodiment 3. is as described in the embodiment 1, and different is that food samples is a multielement nutrition honey, and measurement result is lead＜0.15mg/Kg, zinc: 19.32mg/Kg.
Embodiment 4. is as described in the embodiment 1, and different is that food samples is good precious board 100% plain chocolate, and the smart sample 0.5ml that inhales adds nitric acid 1.0ml, hydrogen peroxidase 10 .3ml, and measurement result is lead＜0.15mg/L, mercury＜0.01mg/L.
Embodiment 5. is as described in the embodiment 1, and different is that food samples is bottled Luokou vinegar, and smart persorption is spared sample 1ml, adds nitric acid 0.7ml, and measurement result is plumbous: 0.10mg/L, arsenic＜0.008mg/L.
Embodiment 6. is as described in the embodiment 1, and different is that food samples is the unleaded preserved egg duck of a refreshing red board lime-preserved egg, and measurement result is lead＜0.15mg/Kg, copper: 2.20mg/Kg, zinc: 1.78mg/Kg.
Embodiment 7. is as described in the embodiment 1, and different is that food samples is day rich board Disposable paper cup of profit, and measurement result be a lead: 0.31mg/Kg, arsenic＜0.016mg/Kg.
In sum, micro-wave digestion food samples method agents useful for same amount of the present invention significantly reduces, and blank value is low, and measurement result is accurate; Avoided traditional digestion method to endanger because of a large amount of harmful gas environmental pollutions of using amount of reagent and producing greatly with to experimenter's health; The sample solution that this law is cleared up can be used for measuring various trace elements, macroelement and the rare earth element in the food, has shortened the working time greatly, has improved work efficiency; Economic benefit obviously improves, and has very big use value and promotional value.
Claims (8)
1. the method for a micro-wave digestion food samples comprises and uses microwave dissolver and nitric acid-hydrogen peroxide or nitric acid, it is characterized in that step is as follows:
(1) digestion solution prepares, and takes by weighing the even food samples 0.2～1.0g of solid, semisolid or vegetable oil, perhaps imbitition sample 0.5～3.0ml, place counteracting tank, alcoholic sample discharges water earlier to bathe and removes alcohol, adds the pure red fuming nitric acid (RFNA) 0.5～1.0ml of top grade, places 10～15min; Add pure 30% hydrogen peroxidase 10 of top grade～0.5ml, place 10～15min, add water to 8～15ml;
(2) above-mentioned sample is shaken up gently, adorn appropriate digestion instrument, and put it in the microwave dissolver, clear up, temperature 100-185 ℃, reaction finishes back cooling automatically.
2. the method for micro-wave digestion food samples as claimed in claim 1 is characterized in that, when digestion solution prepares, and vegetable oil amount of samples 0.2～0.43g.
3. the method for micro-wave digestion food samples as claimed in claim 1 is characterized in that, when digestion solution prepares, for the sample of easily clearing up, during with acid amount＜1.0ml, does not add hydrogen peroxide.
4. the method for micro-wave digestion food samples as claimed in claim 1 is characterized in that, when digestion solution prepared, salted vegetables, vegetables or fruit sample added red fuming nitric acid (RFNA) 0.5～1.0ml, 30% hydrogen peroxidase 10 .0～0.3ml.
5. the method for micro-wave digestion food samples as claimed in claim 1 is characterized in that, when digestion solution prepared, fruit juice, vinegar, soy sauce, milk-contained drink or various wine sample added red fuming nitric acid (RFNA) 0.7～1.0ml, 30% hydrogen peroxidase 10 .0～0.3ml.
6. the method for micro-wave digestion food samples as claimed in claim 1, it is characterized in that, when digestion solution prepares, add red fuming nitric acid (RFNA) 0.8～1.0ml for fatty few cake, wheaten food, candy, honey, milk, marine product or each wrapping paper sample, 30% hydrogen peroxidase 10 .3～0.5ml.
7. the method for micro-wave digestion food samples as claimed in claim 1, it is characterized in that, when digestion solution prepares, add red fuming nitric acid (RFNA) 1.0ml, 30% hydrogen peroxidase 10 .5ml for ice cream, ice cream, tealeaves, solid health food, milk powder, bean powder, coffee, meat, fat cake, peanut oil or soya-bean oil sample.
8. the method for micro-wave digestion food samples as claimed in claim 1 is characterized in that, during micro-wave digestion, can divide 2-3 step to finish, and temperature, pressure progressively raise, per step in 3～8min climbing time, be warmed up to fixed temperature.
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