CN104458605A - Method for detecting content of heavy metals in plant sample - Google Patents
Method for detecting content of heavy metals in plant sample Download PDFInfo
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- CN104458605A CN104458605A CN201410612590.3A CN201410612590A CN104458605A CN 104458605 A CN104458605 A CN 104458605A CN 201410612590 A CN201410612590 A CN 201410612590A CN 104458605 A CN104458605 A CN 104458605A
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Abstract
The invention provides a method for detecting content of heavy metals in a plant sample, particularly a method for treating a to-be-detected sample in a sample pretreatment step by using dilute acid. Compared with a national standard method, the dilute acid method has wide application value, is easy and convenient to operate and rapid; and the national standard method is long in extraction time and easy to pollute and lose, and the dilute acid method is easy and wide to popularize. According to the method disclosed by the invention, heavy metal elements in vegetables are analyzed and measured, and the method has great significance for rapidly detecting the heavy metal elements in the vegetables.
Description
Technical field
The present invention relates to analytical chemistry field, relate to plant sample particularly, especially in vegetable sample, detect the method for content of beary metal.
Background technology
Food security is the major issue of current people's common concern, and heavy metal pollution is again one of major issue of food security.Composing environment, vegetables, food pollution and health is had to the objectionable impurities of very large threat.The pollution of Supervise prevention and cure heavy metal has become the hot issue of countries in the world common concern.Along with the arrival of urbanization, process of industrialization, the discharge of municipal domestic waste and Industrial " three Waste " is increasing, the unreasonable use etc. of agricultural chemicals, chemical fertilizer, the serious water, soil, the gas that pollute in region, cause vegetable-growing area ecologic environment to go from bad to worse, cause quality of vegetable to decline.And heavy metal contaminants constantly accumulates, and pass through the transmission amplification of food chain, irreversibly significant impact is produced to the living standards of urban and rural residents, thus high risks is brought to whole ecologic environment and population health.Analyze content of beary metal in plant sample, especially analyze the content of beary metal in the food plants such as vegetables, contributing to people to the heavy metal pollution degree in environment assesses, and contributes to the control of food hygiene.
Analyze the content of beary metal in sample, the general flame atomic absorption spectrometry that adopts is carried out.Being the analytical approach coming based on quantitative tested constituent content to the absorption intensity of the corresponding atomic resonance radiant rays of ultraviolet light and visible-range based on the ground state atom outer-shell electron of gaseous state, is a kind ofly measure the method for specific gaseous atom to the absorption of optical radiation.This method is the mid-50 appearance in last century and a kind of novel instrument analytical method grown up gradually afterwards, and it is widely used in every field such as geology, metallurgy, machinery, chemical industry, agricultural, food, light industry, biological medicine, environmental protection, material science.This method is mainly suitable for trace and trace components analysis in sample.
At present, use flame atomic absorption spectrometry to analyze plant sample, the content of beary metal especially in vegetable sample, generally take the method for red fuming nitric acid (RFNA)-perchloric acid heating to carry out sample pre-treatments.Detect in relevant GB at the vegetables content of beary metal of China, adopt resolution method to carry out the pre-treatment of vegetable sample.But resolution method extraction time is long, easily contaminated samples, easily cause the shortcomings such as sample loss.Meanwhile, in sample pretreatment process, adopt perchloric acid will likely cause flame atomic absorption spectrometry to measure hollow white value be affected, and then directly have influence on the accuracy of measurement result.
Summary of the invention
The object of this invention is to provide the sample-pretreating method in a kind of content of beary metal especially measured for the sample-pretreating method of content of beary metal in flame atomic absorption spectrometry measurement plant sample in vegetable sample, to overcome above technical matters.
As used herein, term " vegetables " refers to can cook, cooks and become food, other plant (belonging to draft) except cereal more.In life indication vegetables, normal and " fruit " is separately discussed.But also normal and fruit is collectively referred to as " vegetables and fruits ".
Though the vegetables about You20Duo Ge section that China generally cultivates, but common some are planted or mutation mainly concentrates on 8 large sections, and it includes but not limited to: (1) Cruciferae comprises radish, turnip, Chinese cabbage (containing Chinese cabbage, Chinese cabbage subspecies), wild cabbage (containing mutation such as cabbage, kohlrabi, cauliflower, broccolis), leaf mustard (containing root Jie dish, potherb mustard mutation) etc.; (2) Carrot family comprises celery, carrot, fennel seeds, Yuan etc.; (3) Solanaceae comprises tomato, eggplant, capsicum (containing pimento mutation); (4) Curcurbitaceae comprises cucumber, cucurbita pepo, pumpkin, winter squash, wax gourd, sponge gourd, bottle gourd, balsam pear, chocho and watermelon, muskmelon etc.; (5) pulse family comprises Kidney bean (containing dwarf bean, Kidney bean mutation of overgrowing), cowpea, pea, broad bean, green soy bean (i.e. soybean), French beans, sword bean etc.; (6) Liliaceae comprises leek, shallot, onion, garlic, leek, day lily (i.e. day lily), asparagus (asparagus), lily etc.; (7) chrysanthemum material comprises lettuce (containing butter-head lettuce, curled lettuce mutation), asparagus lettuce, crowndaisy chrysanthemum, burdock, jerusalem artichoke, globe artichoke etc.; (8) Chenopodiaceae comprises spinach, beet (containing common beet, beta vulgaris mutation) etc.
From edible plant organ, vegetables comprise following classification:
(1) root vegetables: the vegetables being product organ with the root of hypertrophy belong to this class, as 1. fleshy root---with the loose main root of seed base-root growth for product, as windproof in radish, carrot, root-mustard, turnip, turnip, horseradish, America etc.; 2. block root class---expand for product, as burdock, yam bean, sweet potato, Pueraria lobota etc. with the root that the side root of hypertrophy or vegetative bud occur.
(2) stem dish class: the vegetables being product with the stem of hypertrophy, as: 1. fleshy stem class-mono-is with the aerial stem of plant of hypertrophy for product, has asparagus lettuce, wild rice stem, Stem lettuce, kohlrabi (kohlrabi) etc.; 2. tender stem class---with the tender shoots sprouted for product, as asparagus, bamboo shoots, Chinese toon etc.; 3. tubers---with the stem tuber of hypertrophy for product, as potato, jerusalem artichoke, Chinese artichoke, silver bar dish etc.; 4. tubers---with the rhizome of hypertrophy for product, as lotus rhizome, ginger, assist lotus etc.; 5. corm kind---with the bulb of underground for product, as arrowhead, taro, water chestnut etc.
(3) leaf vegetables: the vegetables being product with fresh and tender blade and petiole, as: 1. common leaf vegetables---pakchoi, leaf mustard, Wuta-tsai, a kind of sedge dish, cabbage mustard, shepherd's purse, spinach, three-coloured amaranth, New Zealand spinach, foliage heet, lettuce, crowndaisy chrysanthemum, celery etc.; 2. balling leaf vegetables---cabbage, Chinese cabbage, butter-head lettuce, envelopped senvy etc.; 3. pungent fragrant leaf vegetables---shallot, leek, shallot, fennel, coriander etc.; 4. bulb class---expanded by leaf sheath base and form bulb, as onion, garlic, recklessly green onion, lily etc.
(4) flower vegetables: with floral organ or fertile tender spray for product, as day lily, globe artichoke, cauliflower, purple tsai-tai, cabbage mustard etc.
(5) fruit vegetables: with fruit and seed for product, as: 1. Peponidium class---pumpkin, cucumber, watermelon, muskmelon, wax gourd, sponge gourd, balsam pear, serpent melon, chocho etc.; 2. berries---tomato, capsicum, eggplant; 3. pod class---Kidney bean, cowpea, sword bean, pea, broad bean, green soy bean etc.; 4. assorted fruit---corn, strawberry, water caltrop, gumbo etc.
Particularly, the invention provides following technical scheme:
In one aspect of the invention, provide a kind of method detecting content of beary metal in plant sample, it is characterized in that, the method comprises carries out pretreated step by vegetable sample, and described pre-treatment step comprises and being shredded by the plant sample after weighing, add watery hydrochloric acid, cool and carry out constant volume after being heated to all dissolvings; Preferably, described plant sample is selected from the root of plant, stem, leaf, flower, fruit and seed; More preferably, described plant sample is selected from stem and leaf.
In the present invention one is preferred, described plant sample is vegetable sample; Preferably, described vegetables are selected from pakchoi, cauliflower and leek; More preferably, described vegetables are pakchois; Again more preferably, described vegetable sample is fresh vegetables sample.
In the present invention one is preferred, the concentration of described watery hydrochloric acid is 2 ~ 8mol/L; Preferably, the concentration of described watery hydrochloric acid is 6mol/L.
In the present invention one is preferred, the mass volume ratio of plant sample and watery hydrochloric acid is 1:5 ~ 20 grams per milliliter; Preferably, described mass volume ratio is 1:10 grams per milliliter.
In the present invention one is preferred, described heating steps is for boiling heating 5 ~ 30 minutes, such as 10-20 minute, 15 minutes particularly; Preferably, described heating steps carries out on adjustable closed electric furnace or electric hot plate.
In the present invention one is preferred, described constant volume carries out to 100mL according to every 1 ~ 10 gram of plant sample constant volume; Preferably, carry out to 100mL according to every 2 grams of plant sample constant volumes.
In a specific embodiment of the present invention, 2.0g vegetable sample adds 20ml watery hydrochloric acid and extracts, after boiling, and constant volume 100ml, centrifuging and taking supernatant.Those skilled in the art should know, and the main heavy metal concentration size per sample of w/v of constant volume determines, if find that heavy metal concentration is too high, also can do certain dilution.
In the present invention one is preferred, it is characterized in that, described method comprises the step using Flame Atomic Absorption Spectrometry spectrophotometer to carry out element determination, and heavy metal element to be measured is one or more of Cu, Cd and Zn; Preferably, flame pattern is air acetylene.
In the present invention one is preferred, the condition of described element determination is: when heavy metal is Cu, and measurement wavelength is 324.8nm, and lamp current is 4mA, and slit width is 0.5nm, gas flow is 1.1L/ minute, and combustion gas is highly 7 centimetres; When heavy metal is Cd, measurement wavelength is 228.8nm, and lamp current is 4mA, and slit width is 0.5nm, gas flow is 1.2L/ minute, and combustion gas is highly 7 centimetres; And heavy metal is when being Zn, measurement wavelength is 213.9nm, and lamp current is 8mA, and slit width is 0.5nm, gas flow is 1.2L/ minute, and combustion gas is highly 7 centimetres.
In the present invention one is preferred, described method also comprises use heavy metal standard model liquid Flame Atomic Absorption Spectrometry spectrophotometer and obtains typical curve and regression equation, and according to the content of beary metal in typical curve and regression equation calculation sample.
Technical scheme of the present invention brings following advantage:
(1) measured the comparison of Heavy Metals In Vegetables element by diluted acid method and National Standard Method, can find out that diluted acid method has more widely used value than National Standard Method, diluted acid method is easy and simple to handle, fast, National Standard Method extraction time is long, easily pollutes, loss, diluted acid method is more easily extensively promoted.
(2) methods analyst of the present invention measures Heavy Metals In Vegetables element, detects significant fast to vegetables heavy metal element.
(3) precision of diluted acid method measurement result is higher than the precision of National Standard Method measurement result, and the measurement result precision of some heavy metal as Cu, Cd etc. will far above National Standard Method.
(4) experimental result adding standard specimen survey time yield by heavy metal element shows, the recovery of diluted acid method is higher than National Standard Method, illustrates that Thinner acid method is feasible, and National Standard Method can be replaced to measure the content of some heavy metal element in vegetables.
Embodiment
the pre-treatment of embodiment 1 vegetable sample
Chemical reagent:
Potassium dichromate (spectroscopic pure, purchased from Beijing Chemical Plant);
Manganese sulfate (analyzing pure, purchased from Beijing Chemical Plant);
Zinc sulfate (analyzing pure, purchased from Beijing Chemical Plant);
Cadmium sulfate (analyzing pure, purchased from Beijing Chemical Plant);
Copper sulphate (analyzing pure, purchased from Beijing Chemical Plant);
Concentrated hydrochloric acid (analyzing pure, purchased from Beijing Chemical Plant);
Red fuming nitric acid (RFNA) (analyzing pure, purchased from Beijing Chemical Plant);
Perchloric acid (top grade is pure, purchased from Beijing Chemical Plant).
Vegetable sample:
Fresh pakchoi (Chinese cabbage, the shoot of crucifer green vegetables Brassica chinensis L.), Hefei City two is buied Li Jie food market at random.
Experimental apparatus
Stainless steel temp .-adjustable electric hot plate (instrument company of SAST of Longkou, Shandong Province city produces, model: TP-3, and power is 700W);
Adjustable closed electric furnace (power is 1KW);
Electronic balance (model: FA1104 type, Shanghai balance equipment factory);
Electric heating constant-temperature blowing drying box (model: DHG-9070A type, the grand experimental facilities company limited of upper Nereid).
With water, the earth impurity on fresh vegetables is cleaned, dry surface moisture.
Test group (diluted acid method) 1: accurately take the fresh sample of 2.0g and shred in 50ml conical flask, add the hydrochloric acid of 20ml 6mol/L, on adjustable closed electric furnace, heating is boiled and is taken off cooling in 15 minutes, and filter and move in 100ml volumetric flask, after constant volume, centrifuging and taking supernatant is to be measured.Repeat 3 times.
Wherein, described fresh sample is the whole edible parts after removing root, whole strain pakchoi is shredded the rear fresh sample of 2.0g that accurately takes in 50ml conical flask.
Embodiment below the present invention, if not otherwise indicated, the diluted acid method vegetable sample used is the vegetable sample prepared according to the method for test group (diluted acid method) 1.
Blank group 1: get 20ml 6N hydrochloric acid and be placed in 50ml conical flask, adjustable closed electric furnace heats 15 minutes, takes off cooling, filters and moves in 100ml volumetric flask, constant volume.
Control group (according to national standard method): accurately take 2g fresh sample (preparation method is with identical) above in 50ml conical flask, add 20ml red fuming nitric acid (RFNA), on electric hot plate ebuillition of heated clear up about 2 little be faint yellow up to solution, then add 5ml perchloric acid.Continue heating, be evaporated near dry, have a large amount of white cigarette to emerge, take off cooling, constant volume is to 100mL and filter.Repeat 3 times.
Blank group 2: get 20ml red fuming nitric acid (RFNA) and be placed in 50ml conical flask, heating and decompose about 2 is little on electric hot plate is faint yellow up to solution, then adds 5ml perchloric acid.Continue heating, be evaporated near dry, have a large amount of white cigarette to emerge, take off cooling, move in 100ml volumetric flask, constant volume, filter
Prepare test group (diluted acid method) 2-5 according to following test parameters, test the effect of the diluted acid method under other test conditions.
Test group (diluted acid method) 2: accurately take the fresh sample of 2.0g and shred in 50ml conical flask, add the hydrochloric acid of 20ml 2mol/L, on adjustable closed electric furnace, heating is boiled and is taken off cooling in 30 minutes, and filter and move in 100ml volumetric flask, after constant volume, centrifuging and taking supernatant is to be measured.Repeat 3 times.
Test group (diluted acid method) 3: accurately take the fresh sample of 2.0g and shred in 50ml conical flask, add the hydrochloric acid of 10ml 6mol/L, on adjustable closed electric furnace, heating is boiled and is taken off cooling in 20 minutes, and filter and move in 100ml volumetric flask, after constant volume, centrifuging and taking supernatant is to be measured.Repeat 3 times.
Test group (diluted acid method) 4: accurately take the fresh sample of 2.0g and shred in 50ml conical flask, add the hydrochloric acid of 40ml 8mol/L, on adjustable closed electric furnace, heating is boiled and is taken off cooling in 5 minutes, and filter and move in 100ml volumetric flask, after constant volume, centrifuging and taking supernatant is to be measured.Repeat 3 times.
Test group (diluted acid method) 5: accurately take the fresh sample of 2.0g and shred in 50ml conical flask, add the hydrochloric acid of 20ml 6mol/L, on adjustable closed electric furnace, heating is boiled and is taken off cooling in 10 minutes, and filter and move in 100ml volumetric flask, after constant volume, centrifuging and taking supernatant is to be measured.Repeat 3 times.
embodiment 2: the atomic absorption spectroscopy of vegetable sample
The atomic absorption spectrophotometer (AAS) used is U.S. Thermo Elenent SOLAAR M5 type.
Process in processing sample and Metalization of skin, flame pattern: air acetylene, condition is as follows
Table 1: element instrument measuring condition
Configure Cu, Zn, Cd 1000 standard reserving solution of μ g/mL respectively.
Standard solution preparation is carried out according to following method:
(1) Cu takes Ni metal (high-purity) 0.5000g and is dissolved in a small amount of nitric acid, evaporate to dryness in water-bath, adds 5ml hydrochloric acid evaporate to dryness again, is diluted to 500ml with 1mol/L dissolving with hydrochloric acid, then the standard reserving solution of 1000mg/L Cu.
(2) Zn: take Metal Zn (AR) 0.5000g, with a small amount of 6N hydrochloric acid to 500ml, obtains 1000mg/L standard reserving solution.
(3) accurately take cadmium sulfate 2.2364g, dissolve, constant volume 500ml.This solution is 1000mg/LCd standard reserving solution.
The each heavy metal species standard model liquid flame method configured is drawn typical curve and regression equation, and regression equation is in table 2.
Each heavy metal species standard model liquid prepares sample as follows: draw above-mentioned standard reserving solution Cu:4.0ml, Zn:3.0ml respectively; Cd1.0ml constant volume is in 100ml volumetric flask.Draw this liquid preparation series standard more respectively, Cu:0.0 ~ 4.8mg/L, Zn:0.0 ~ 3.6mg/L, Cd:0.0 ~ 1.2mg/L, condition is as table 1.
The regression equation of table 2:Cu, Cd and Zn and correlativity
The related coefficient of each typical curve is all more than 0.98 as seen from Table 2, meets the requirement analyzing quality control.Wherein, Y is absorbance, and X is each heavy metal concentration of solution (unit is mg/L), and blank is deducted.
The various samples prepared according to embodiment 1 are measured according to the method for table 1, the value that is absorbed result.Its empty is deducted.Data show, and the sample of test group (diluted acid method) the 1-5 group prepared according to method of the present invention all records the absorption value close with National Standard Method, and the absorption value ratio of test combinations National Standard Method is all between 0.86-1.05 particularly.This shows according to the standby sample of diluted acid legal system of the present invention in the pretreatment process of vegetable sample, obtains the result similar to National Standard Method.
Below show the result of test group (diluted acid method) 1 and National Standard Method, other data do not show.
The ratio of table 3 two kinds of method measured values
As can be seen from Table 3, this law and National Standard Method ratio C u, Zn and Cd reach 0.87-0.94, and for the content measuring this 3 heavy metal species in vegetables, Thinner acid method can substitute National Standard Method.
By Cu, Zn and Cd in testing sample (diluted acid method 1 and the National Standard Method) working sample of preparation in embodiment 1, with the precision of inspection method, the results are shown in Table 4 (wherein σ is standard deviation).
Table 4 method precision is tested
As can be seen from Table 4, Cu is recorded by diluted acid method, Zn, little compared with the standard deviation of National Standard Method measured value all respectively with the standard deviation of Cd value, illustrate that Thinner acid method precision can reach and be better than National Standard Method, mainly because Thinner acid method method is easy, experimental procedure is few, thus reduces accidental error.
embodiment 3: Thinner acid method and the National Standard Method recovery compare
In unknown sample, add each heavy metal solution of certain concentration known, measure the heavy metal concentration before and after mark-on respectively, the recovery of computing method, the i.e. recovery=C
after mark-on-C
before mark-on)/C
add scalar× 100%, result is as table 5.Recovery testu carries out according to following method: get equivalent vegetable sample two parts (preparing according to the method for embodiment 1), a copy of it adds a certain amount of standard reserving solution Cu, Zn, Cd (preparing according to the method for embodiment 2), portion does not add in addition, same method processing sample.Record content of beary metal, calculate its recovery, compare the recovery of National Standard Method and diluted acid method (carrying out according to the method for diluted acid method 1 group) respectively.
Table 5: the recovery of Thinner acid method and GB extraction method compares
The recovery of diluted acid method mensuration Heavy Metals In Vegetables element is higher as seen from Table 5, and generally between 91%-104%, reliable results, meets the requirements, and the recovery of National Standard Method is between 89%-112%.Can find out from recovery result adopts National Standard Method to measure Heavy Metals In Vegetables element, heavy metal element is easily made to lose, make measurement result less than normal, and employ perchloric acid in National Standard Method, the purity of perchloric acid is very large on the impact of blank value, directly have influence on the accuracy of measurement result, so rare acidity extraction is feasible.
Claims (9)
1. detect a method for content of beary metal in plant sample, it is characterized in that, the method comprises carries out pretreated step by vegetable sample, and described pre-treatment step comprises and being shredded by the plant sample after weighing, add watery hydrochloric acid, rear cooling is boiled in heating, and carries out constant volume; Preferably, described plant sample is selected from the root of plant, stem, leaf, flower, fruit and seed; More preferably, described plant sample is selected from stem and leaf.
2. method according to claim 1, is characterized in that, described plant sample is vegetable sample;
Preferably, described vegetables are selected from pakchoi, cauliflower and leek;
More preferably, described vegetables are pakchois;
Again more preferably, described vegetable sample is fresh vegetables sample.
3. the method described in claim 1 or 2, is characterized in that, the concentration of described watery hydrochloric acid is 2 ~ 8mol/L; Preferably, the concentration of described watery hydrochloric acid is 6mol/L.
4. the method described in claim 1 or 2, is characterized in that, the mass volume ratio of plant sample and watery hydrochloric acid is 1:5 ~ 20 grams per milliliter;
Preferably, described mass volume ratio is 1:10 grams per milliliter.
5. the method described in claim 1 or 2, is characterized in that, described heating steps such as, for boiling heating 5-30 minute, 10-20 minute, 15 minutes particularly;
Preferably, described heating steps carries out on adjustable closed electric furnace or electric hot plate.
6. the method described in claim 1 or 2, is characterized in that, described constant volume carries out to 100mL according to every 1 ~ 10 gram of plant sample constant volume; Preferably, carry out to 100mL according to every 2 grams of plant sample constant volumes.
7. the method described in claim 1 or 2, is characterized in that, described method comprises the step using Flame Atomic Absorption Spectrometry spectrophotometer to carry out element determination, and heavy metal element to be measured is one or more of Cu, Cd and Zn;
Preferably, flame pattern is air acetylene.
8. method according to claim 7, is characterized in that, the condition of described element determination is:
When heavy metal is Cu, measurement wavelength is 324.8nm, and lamp current is 4mA, and slit width is 0.5nm, gas flow is 1.1L/ minute, and combustion gas is highly 7 centimetres;
When heavy metal is Cd, measurement wavelength is 228.8nm, and lamp current is 4mA, and slit width is 0.5nm, gas flow is 1.2L/ minute, and combustion gas is highly 7 centimetres; And
When heavy metal is Zn, measurement wavelength is 213.9nm, and lamp current is 8mA, and slit width is 0.5nm, gas flow is 1.2L/ minute, and combustion gas is highly 7 centimetres.
9. the method described in claim 7 or 8, it is characterized in that, described method also comprises use heavy metal standard model liquid Flame Atomic Absorption Spectrometry spectrophotometer and obtains typical curve and regression equation, and according to the content of beary metal in typical curve and regression equation calculation sample.
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| CN109358015A (en) * | 2018-12-20 | 2019-02-19 | 利民化工股份有限公司 | Zinc-manganese content assaying method in a kind of generation gloomy class product |
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