CN105452841A - Sample pre-treatment method for measuring the quantity of toxic elements in agricultural produce samples - Google Patents
Sample pre-treatment method for measuring the quantity of toxic elements in agricultural produce samples Download PDFInfo
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- 238000002203 pretreatment Methods 0.000 title abstract description 8
- 231100000701 toxic element Toxicity 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 212
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 40
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 34
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011701 zinc Substances 0.000 claims abstract description 34
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 34
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229920002472 Starch Polymers 0.000 claims abstract description 20
- 239000008107 starch Substances 0.000 claims abstract description 20
- 235000019698 starch Nutrition 0.000 claims abstract description 20
- 108090000790 Enzymes Proteins 0.000 claims abstract description 19
- 102000004190 Enzymes Human genes 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 244000046052 Phaseolus vulgaris Species 0.000 claims abstract description 11
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims abstract description 11
- 235000013339 cereals Nutrition 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 239000011651 chromium Substances 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 239000011133 lead Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims description 79
- 241000196324 Embryophyta Species 0.000 claims description 20
- 229940088598 enzyme Drugs 0.000 claims description 18
- 244000068988 Glycine max Species 0.000 claims description 11
- 235000010469 Glycine max Nutrition 0.000 claims description 11
- 235000003434 Sesamum indicum Nutrition 0.000 claims description 10
- 230000007704 transition Effects 0.000 claims description 9
- 102000013142 Amylases Human genes 0.000 claims description 5
- 108010065511 Amylases Proteins 0.000 claims description 5
- 108010059892 Cellulase Proteins 0.000 claims description 5
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- 102000035195 Peptidases Human genes 0.000 claims description 5
- 108091005804 Peptidases Proteins 0.000 claims description 5
- 229940106157 cellulase Drugs 0.000 claims description 5
- 229940111205 diastase Drugs 0.000 claims description 5
- 235000019833 protease Nutrition 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 240000002791 Brassica napus Species 0.000 claims description 3
- 235000004977 Brassica sinapistrum Nutrition 0.000 claims description 3
- 240000008620 Fagopyrum esculentum Species 0.000 claims description 3
- 235000009419 Fagopyrum esculentum Nutrition 0.000 claims description 3
- 235000021307 Triticum Nutrition 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 244000000231 Sesamum indicum Species 0.000 claims 1
- 244000098338 Triticum aestivum Species 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 47
- 230000001131 transforming effect Effects 0.000 abstract 2
- 238000011084 recovery Methods 0.000 description 41
- 235000021329 brown rice Nutrition 0.000 description 29
- 230000008033 biological extinction Effects 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 24
- 150000004678 hydrides Chemical class 0.000 description 24
- 238000013459 approach Methods 0.000 description 15
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 12
- 239000004743 Polypropylene Substances 0.000 description 10
- 241000207961 Sesamum Species 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 210000000498 stratum granulosum Anatomy 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 240000000359 Triticum dicoccon Species 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 240000001417 Vigna umbellata Species 0.000 description 1
- 235000011453 Vigna umbellata Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 235000019784 crude fat Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/10—Starch-containing substances, e.g. dough
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
Landscapes
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Provided is a method with which it is possible to simply, accurately, rapidly and at a high extraction rate carry out on-site the pre-treatment of samples when measuring the quantity of toxic elements in agricultural produce samples of cereals, beans or seeds. This is a pre-treatment method for samples for measuring of the quantity of at least one element selected from a group consisting of cadmium, arsenic, zinc, manganese, copper, lead and chromium, in agricultural produce samples selected from cereals, beans and seeds, characterized by containing: (i) a step in which the sample is coarsely ground; (ii) a step in which water is added to the coarsely ground sample and heated, transforming the [beta] starch contained in the sample into [alpha] starch; (iii) a step in which an enzyme is added to the sample, transforming the [alpha] starch in the sample into sugar; (iv) a step in which hydrochloric acid is added to the sample to extract the elements being measured in the sample; and (v) a step in which solids are removed from the extracted liquid. The rough grinding of the sample is preferably carried out when measuring the moisture content of the sample, and the heating of the roughly-ground sample is preferably carried out by microwave.
Description
Technical field
The present invention relates to a kind of pre-treating method of sample of the amount for measuring the harmful elements such as cadmium in the crop sample such as rice, soybean, sesame at the scene, relate to a kind of compared with method in the past, make the method that the time of operation and time reduce, the extraction ratio of mensuration element is improved especially.
Background technology
In recent years, from the environmental consciousness on societies such as environmental preservations, consider the raising of the care of the impact of health, the accumulation with the environmental pollutants of the various scenes of industry, life becomes problem.In environmental pollutants, the harmful elements such as cadmium cause serious problem due to its toxicity all the time, and the amount understanding harmful element contained in crops is very important.
The amount of harmful element contained in crops uses the analytical equipments such as ICP emission spectroanalysis device, atom extinction photometer to measure usually.Such as, in the analysis of the harmful elements such as the cadmium contained by the crops of Agriculture, Forestry and Fisheries Ministry, also adopt the mensuration utilizing ICP emission spectroanalysis device, atom extinction photometer.
But the mensuration employing these equipment not only needs the analytical equipment of very high price, special pre-treatment, and needs long processing time and labour.In addition, can not measure near the scene, need sample to deliver to and be provided with arranging and measuring at that of analytical equipment.
On the other hand, as the method for measuring can carrying out the cadmium amount of crops near the scene, patent documentation 1 is proposed.The method is compared with above-mentioned method, can measure at short notice, but when sample be grain class, beans or plant subclass, need to carry out Crushing of Ultrafine when pre-treatment with mill (millser), the washing time and the fine time that are used for mill when the mensuration of Multi-example are long, therefore there is the problems such as the faults frequent generation of mill.In addition, in the method, improved the extraction carrying out cadmium with the contact rate of hydrochloric acid by the Crushing of Ultrafine of sample, but the movability of the cadmium ion from plant cell structures can not be guaranteed fully, therefore, there is the problem of the significantly few sample often producing cadmium extracted amount.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2010-133949 publication
Summary of the invention
Invent problem to be solved
The present invention invents in view of the problem points of above-mentioned conventional art, its object is to, provide a kind of can easy at the scene and carry out the amount of the element measuring grain class, beans or plant cadmium, arsenic, zinc, manganese, copper, lead and/or chromium in the crop sample of subclass in short time well with high extraction ratio precision time the method for pre-treatment of sample.
In order to solve the means of problem
The present inventor to achieve these goals, for can not carrying out utilizing the Crushing of Ultrafine of mill and being concentrated on studies with the pre-treating method of fully extraction and determination element by easy method, found that, so that the mode of the comminutor used in the moisture content determining device that uses when the moisture rate of sample measures can be utilized by sample residence in coarse crushing, water is added wherein and heat, thus be α starch by β starch transition, and then by the interpolation of enzyme by α starch transition for sugar and after being set to filtrable liquid condition, utilize hydrochloric acid extraction to measure element and filter and do not need composition, the fine problem utilizing mill can be eliminated, also can realize the extraction ratio of the high mensuration element from sample simultaneously, until complete the present invention.
That is, the present invention has the formation of following (1) ~ (7).
(1) a kind of pre-treating method of sample, it is for measuring the amount of at least one element in the group that is selected from and is made up of cadmium, arsenic, zinc, manganese, copper, lead and the chromium in the crop sample selected from grain class, beans or plant in subclass, it is characterized in that, comprising:
The operation of (i) coarse crushing sample,
(ii) water be added into the sample through coarse crushing and heat, β starch transition contained in sample being become the operation of α starch,
(iii) enzyme is added into sample and by the operation of the α starch transition saccharogenesis in sample,
(iv) hydrochloric acid be added into sample and extract the operation of the mensuration element in sample, and
V () is from the operation of the liquid removing solid extracted.
(2) method as described in (1), is characterized in that, the coarse crushing of sample is the coarse crushing carried out when the moisture rate of sample measures.
(3) method as described in (1) or (2), is characterized in that, utilizes microwave to carry out the heating of the sample after coarse crushing.
(4) method as described in any one of (1) ~ (3), is characterized in that, uses diastase, proteinase and cellulase as enzyme.
(5) method as described in any one of (1) ~ (4), is characterized in that, vibrate after adding enzyme to sample and after adding hydrochloric acid sample respectively.
(6) method as described in any one of (1) ~ (5), it is characterized in that, grain class is rice, wheat or buckwheat, beans is soybean or peanut, and planting subclass is sesame or rapeseed.
(7) tool box, it comprises utensil for implementing the method described in any one of (1) ~ (6) and reagent.
Invention effect
Pre-treating method of the present invention, in order to improve and the contact rate of hydrochloric acid and not Crushing of Ultrafine sample, therefore not need to use the atomizers such as mill, therefore, does not have the careful washing of atomizer or the burden of switching cost.Enough owing to replacing Crushing of Ultrafine with coarse crushing, therefore usually can be directly used in the coarse crushing sample when moisture rate carried out in crops measures, the weighing of sample, the time of pulverizing can be omitted.In addition, as its result, overall minute is short, and cost of determination is also low.In addition, by measuring the effective destruction of the plant cell structures of element to the moisture of plant cell structures and constraint, the movability measuring element is high, and chloro-complexization can be utilized to extract fully.Therefore, the extraction from the mensuration element of sample can fully be carried out, and estimating precision is high.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the step representing the pre-treating method of the present invention used in embodiment.
Fig. 2 is the schematic diagram of the step representing the previous methods B used in embodiment.
Embodiment
The pre-treating method of sample when the present invention is the amount of the specific harmful element measuring specific crop sample, it consists essentially of (i) coarse crushing operation, the interpolation of (ii) water of sample and heating process, (iii) enzyme add operation, (iv) hydrochloric acid adds operation and (v) solid removal step.
Crop sample as the object of method of the present invention is selected from grain class, beans or kind subclass; these crops are owing to being protected by cellulose layer on surface; therefore have following feature: under the state when directly gathering in the crops, the treating fluids etc. such as hydrochloric acid cannot reach inner stratum granulosum fully.As grain class, rice, wheat, buckwheat etc. can be enumerated, as beans, soybean, red bean, peanut etc. can be enumerated, as kind of a subclass, can sesame, rapeseed etc. be enumerated.
Mensuration element as the object of method of the present invention is selected from least one element in the group be made up of cadmium, arsenic, zinc, manganese, copper, lead and chromium.These elements bring injurious effects to human body, therefore need the content monitored before circulation in crops.
In (i) of the present invention coarse crushing operation, the sample of crops that should be determined carries out coarse crushing.At this, coarse crushing refers to that each crushing piece of sample is can confirm such pulverizing by visual, as long as sample is divided at least two panels, is then abundant.Do not require that each crushing piece of sample is not such by visual confirmation Crushing of Ultrafine.If this is because be divided at least two panels, then the stratum granulosum of the inside of sample exposes, and treating fluid reaches stratum granulosum.As the method for coarse crushing, be not particularly limited, but such as can enumerate the method for beaing with mallet, hammer etc., crushing by hard object.Or, also directly can utilize the sample through coarse crushing when the moisture rate of crop sample measures.Thereby, it is possible to omit the time etc. of coarse crushing or weighing.When being completed by coarse crushing by sample as method of the present invention, compared with Crushing of Ultrafine, complete the washing of comminutor with air gun etc. at short notice easily, the handling member number hourly when processing many samples increases significantly.In addition, if for coarse crushing, then do not use mill, therefore do not need to be considered as fault or the exchange of the mill of shorter device in serviceable life.
Adding at (ii) of the present invention water and in heating process, water be added into the sample through coarse crushing and heat, is α starch by β starch transition contained in sample.Sample through coarse crushing is the β starch that water wettability is low in the state of large crushing piece, and hydrochloric acid extraction therefore can not be utilized to measure element.Therefore, in this operation, by water is added into coarse crushing sample and heating with boiling sample, be α starch and colloidization by β starch transition.Thus, the water wettability of sample uprises, utilize hydrochloric acid fully extraction and determination element become possibility.The water added can be common tap water, but preferably uses ion exchange water.The water yield of adding is more than the isometric(al) of sample weight.The water yield does not have the upper limit, if but too much, then the amount of removing after increases.As heating means, be not particularly limited, the container being added with water in the sample directly can be heated, but easy and effectively by using the microwave such as electric stove to carry out heating, because of but preferably.When being heated by microwave, such as, under 500W, carry out 30 seconds left and right rows be fully.When scene such does not in the wild have a firing equipment, can utilize by adding lime chloride, calcium carbonate and the heat of solution that produces heats.
Add in operation at (iii) of the present invention enzyme, enzyme is added into sample and is sugar by the α starch transition in sample.Sample in the interpolation of aforesaid (ii) water and heating process becomes colloidal (gel), therefore in this state, can not filter afterwards.Therefore, in this operation, by the interpolation of enzyme, the starch in sample is decomposed into sugar, makes it become rustlingly rustlingly liquid.In order to make enzyme play its ability, preferably add under neutral territory substantially.In addition, after adding enzyme to sample, in order to make enzyme soak into sample fully, preferably vibrate sample.As enzyme, be just not particularly limited as long as above-mentioned purpose can be realized, but such as can use diastase, proteinase and cellulase.Diastase has effect starch being decomposed into sugar, and proteinase and cellulase have the effect of the chaff of breakdown surface layer when sample is such as rice.As long as the addition of enzyme carries out being fully to the transformation of sugar, can be more than the isometric(al) of sample weight usually.
Add in operation at (iv) of the present invention hydrochloric acid, hydrochloric acid is added into sample and extracts the mensuration element in sample.As hydrochloric acid, the hydrochloric acid solution of the concentration of 0.002 ~ 2M, more preferably 0.05 ~ 0.5M preferably can be used.The usage ratio of hydrochloric acid solution is generally 5 ~ 100 capacity % of sample, is more preferably 10 ~ 50 capacity %.If use amount is very few, then can not form enough chloro-complexs, if use amount is too much, then the snotter in sample increases.Hydrochloric acid solution can be added directly to sample, or also sample can be impregnated in hydrochloric acid solution.In a word, as long as adopt hydrochloric acid can soak into the method for sample fully.No matter adopt which kind of method, in order to make hydrochloric acid soak into sample fully, preferably vibrate sample intensely.By this operation, the mensuration element from the movement in sample forms chloro-complex.Particularly in the operation of aforesaid (i) ~ (iii), restrained mensuration element in the sample all moves in the mode can reacted with chlorine, therefore can form complex compound for whole mensuration elements.
In (v) of the present invention solid removal step, by filter or centrifuging etc. from the liquid be extracted except deproteinize, crude fat, ash grade solid.Filtration can use the filter paper of such as No.2, and centrifuging can be carried out under the usual setting of centrifugal separator.Thus, the applicability of amount to determinator measuring element improves significantly.
The amount of element can be measured by any one method known through comprising the pre-treating method of the operation of above-mentioned (i) ~ (v) of the present invention and the sample prepared.As assay method, such as can use ICP method, fluorescent X-ray method, immunoassay, voltammetry or light absorption method etc., specifically can use atomic absorption analysis (AAS), inductively coupled plasma atom luminesceence analysis (ICP-AES), inductivity coupled plasma mass spectrometry analysis (ICP-MS) etc.
Embodiment
Below, specifically confirmed by the effect of embodiment to the pre-treating method of sample of the present invention.Be explained, the record of embodiment is only merely enumerated in order to the understanding of inventing, and the present invention is not by any restriction of these embodiments.
Embodiment 1
By 50 brown rice sample near infrared moisture meters, (Co., Ltd. ケ Star ト scientific research is made, rice wheat moisture meter SP-1D3 type) carry out coarse crushing after, make the extract of method of the present invention according to following extraction operation (pre-treating method of the present invention).
Extract operation:
I the brown rice sample 1g having carried out coarse crushing with moisture meter is put into PP bottle (polypropylene vial) by (), then add ion exchange water 2.5mL ((i) with reference to Fig. 1).
(ii) PP bottle is not put into micro-wave oven lid lid, after heating about 30 seconds with 500W, add enzyme solutions (the mixed in equal amounts solution of diastase, proteinase and cellulase: 10 % by weight concentration) 2.5mL and cover the lid of PP bottle, under on hand, vibrating about 10 seconds ((ii) reference of Fig. 1) lightly.
(iii) take the lid of PP bottle, add 0.2N hydrochloric acid solution 5mL, cover lid tightly, under on hand, vibrate about 1 minute ((iii) with reference to Fig. 1) intensely subsequently.
(iv) No.2 filter paper is arranged at new PP bottle, the total amount of the solution of (iii) is filtered ((iv) with reference to Fig. 1).
On the other hand, nitric acid is added to 50 identical brown rice samples, hot plate heats about 24 hours, at the end of decomposition, add aquae hydrogenii dioxidi and decompose completely, make extract according to this extraction operation (previous methods A).Be explained, can say that the extraction ratio of the mensuration element of previous methods A is 100%, but due to the long pre-treatment of needs, be therefore the method that cannot use at the scene.This previous methods A as the extraction ratio of the mensuration element of pre-treating method of the present invention Comparative indices and implement.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of the inventive method and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each brown rice sample (specimen coding 1 ~ 50) are shown in following table 1.
As can be known from the results of Table 1, although the sample confirming to obtain with pre-treating method of the present invention can process at short notice, same with the long previous methods A of needs, fully extract the mensuration element of cadmium, manganese, zinc, arsenic.
Comparative example 1
By each sample use for laboratory atomizer (Osaka ケ ミ カ Le Co., Ltd. system of 50 brown rice samples, LABMillserPlus, LM-PLUS) carry out Crushing of Ultrafine, make the extract of previous methods B subsequently according to following extraction operation (previous methods B).
Extract operation:
Brown rice sample 1g after Crushing of Ultrafine is put into PP bottle (polypropylene vial), then adds 0.1N hydrochloric acid 10mL.With hand, this PP bottle is vibrated about 1 minute up and down intensely, subsequently this solution is put into the new PP bottle being provided with No.2 filter paper and carry out total amount filtration (with reference to Fig. 2).
On the other hand, from 50 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to aforesaid previous methods A.
Then, to the extract made according to previous methods B and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with previous methods B relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that expression previous methods B obtains is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the previous methods B for each brown rice sample (specimen coding 1 ~ 50) are shown in following table 2.
As can be known from the results of Table 2, in previous methods B, cannot obtain sufficient extraction efficiency, the extraction therefore sometimes produced as the specimen coding 13 and 17 of table 2 is not enough.In addition, in previous methods B, although extraction operation is simple compared with previous methods A, but, if each sample needs the Crushing of Ultrafine time of about 2 minutes in the Crushing of Ultrafine operation of each sample, then in order to prevent the engine overheat of comminutor, every Crushing of Ultrafine 5 samples need the natural cool time of about 15 minutes, therefore, the pulverization process of 50 samples needs the time adding up to about 4 hours.On the other hand, in such pre-treating method of the present invention as described in Example 1, in crushing operation, need the time hardly, therefore when process 50 samples, compared with previous methods B, the time of more than 3 hours can be shortened.
Embodiment 2
20 soybean sample agate mortars beaten and carries out coarse crushing, making the extract of the inventive method subsequently similarly to Example 1 according to pre-treating method of the present invention.
On the other hand, from 20 identical soybean samples, the extract of previous methods A is made similarly to Example 1 according to aforesaid previous methods A.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of the inventive method and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each soybean sample (specimen coding 1 ~ 20) are shown in following table 3.
As can be known from the results of Table 3, although the sample confirming to obtain with pre-treating method of the present invention can process at short notice, in the same manner as the long previous methods A of needs, the mensuration element of cadmium, manganese, zinc, arsenic is fully extracted.
Comparative example 2
By each sample use for laboratory atomizer (Osaka ケ ミ カ Le Co., Ltd. system of 20 soybean samples, LABMillserPlus, LM-PLUS) Crushing of Ultrafine is carried out, subsequently using every 10 samples on hot plate roasting about 30 minutes until become brown as sample (annotation: previous methods B soybean measure in, if do not carry out calcination process, then do not carry out Separation of Solid and Liquid by filtering).Operate according to the extraction same with the previous methods B that comparative example 1 is recorded the extract that (wherein, duration of oscillation changes to 30 minutes) makes previous methods B from this sample.
On the other hand, from 20 identical soybean samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to previous methods B and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with previous methods B relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that expression previous methods B obtains is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the previous methods B for each soybean sample (specimen coding 1 ~ 20) are shown in following table 4.
As can be known from the results of Table 4, in previous methods B, cannot obtain sufficient extraction efficiency, the extraction therefore sometimes produced as the specimen coding 11 of table 4 is not enough.In addition, in previous methods B, need further calcination process in operation before extraction, and, the extraction time of each sample also needs about 30 minutes, therefore the process of 20 samples needs total more than 12 hours, compared with pre-treating method of the present invention, needs the processing time of more than 10 hours.
Embodiment 3
20 sesame sample agate mortars beaten and carries out coarse crushing, making the extract of the inventive method subsequently similarly to Example 1 according to the pre-treating method of the inventive method.
On the other hand, from 20 identical sesame samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of the inventive method and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each sesame sample (specimen coding 1 ~ 20) are shown in following table 5.
As can be known from the results of Table 5, although the sample confirming to obtain with pre-treating method of the present invention can process at short notice, in the same manner as the long previous methods A of needs, the mensuration element of cadmium, manganese, zinc, arsenic is fully extracted.
Comparative example 3
By each sample use for laboratory atomizer (Osaka ケ ミ カ Le Co., Ltd. system of 20 sesame samples, LABMillserPlus, LM-PLUS) carry out Crushing of Ultrafine, make the extract of previous methods B subsequently according to previous methods B in the same manner as comparative example 1.
On the other hand, from 20 identical sesame samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to previous methods B and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with previous methods B relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that expression previous methods B obtains is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the previous methods B for each sesame sample (specimen coding 1 ~ 20) are shown in following table 6.
As can be known from the results of Table 5, in previous methods B, cannot obtain sufficient extraction efficiency, the extraction therefore sometimes produced as the specimen coding 5 and 13 of table 6 is not enough.In addition, in previous methods B, although brown rice is identical, extraction operation is simple compared with previous methods A, if but each sample needs the Crushing of Ultrafine time of about 2 minutes in the Crushing of Ultrafine operation of each sample, then in order to prevent the engine overheat of comminutor, every Crushing of Ultrafine 5 samples need the natural cool time of about 15 minutes, and therefore the pulverization process of 20 samples needs the time adding up to about 2 hours.On the other hand, in such pre-treating method of the present invention as described in Example 3, in crushing operation, need the time hardly, therefore compared with previous methods B, can operate the time below 1/2.
Comparative example 4
Use 10 brown rice specimen sample, in the extraction operation of the pre-treating method of the present invention of embodiment 1, do not carry out interpolation and the heating utilizing micro-wave oven shown in (ii) of the water shown in (i), in addition, operate similarly to Example 1, the extract of comparison method A.
On the other hand, from identical brown rice 10 sample, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to comparative approach A and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with comparative approach A relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that obtains of expression comparative approach A is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the comparative approach A for each brown rice sample (specimen coding 1 ~ 10) are shown in following table 7.
Learn from the result of table 7, in comparative approach A, the recovery reduces to heavens, cannot obtain sufficient extraction effect.
Comparative example 5
Use 10 brown rice specimen sample, in the extraction operation of the pre-treating method of the present invention of embodiment 1, do not carry out the interpolation of the enzyme shown in (ii), in addition, operate similarly to Example 1, the extract of comparison method B.
On the other hand, from 10 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to comparative approach B and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with comparative approach B relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that obtains of expression comparative approach B is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the comparative approach B for each brown rice sample (specimen coding 1 ~ 10) are shown in following table 8.
Learn from the result of table 8, in comparative approach B, the recovery reduces to heavens, cannot obtain sufficient extraction effect.
Comparative example 6
Use 10 brown rice specimen sample, in the extraction operation of the pre-treating method of the present invention of embodiment 1, do not carry out the coarse crushing utilizing moisture meter, in addition, operate similarly to Example 1, the extract of comparison method C.
On the other hand, from 10 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to comparative approach C and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the ratio (%) of the amount of the mensuration element obtained with comparative approach C relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery is more close to 100%, then the extract that obtains of expression comparative approach C is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the comparative approach C for each brown rice sample (specimen coding 1 ~ 10) are shown in following table 9.
Learn from the result of table 9, in comparative approach C, the recovery reduces to heavens, cannot obtain sufficient extraction effect.
Embodiment 4
Use 10 brown rice specimen sample, in the extraction operation of the pre-treating method of the present invention of embodiment 1, replace and utilize the coarse crushing of moisture meter and utilize mallet to be split into two halves by brown rice, in addition, operate similarly to Example 1, make the extract of the inventive method.
On the other hand, from 10 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of method of the present invention and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each brown rice sample (specimen coding 1 ~ 10) are shown in following table 10.
As known from Table 10, even if utilize the coarse crushing of mallet, also achieve the recovery of admissible level, also do not see the example showing low-down value, therefore can think, as long as there is the degree of fragmentation of this degree, then there is fully practical possibility.
Embodiment 5
Use 10 brown rice specimen sample, in the extraction operation of the pre-treating method of the present invention of embodiment 1, replace and utilize the coarse crushing of moisture meter and utilize mallet to be divided into by brown rice until about 20, in addition, operate similarly to Example 1, make the extract of the inventive method.
On the other hand, from 10 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to previous methods A.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of each element of cadmium, manganese, zinc, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of method of the present invention and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each brown rice sample (specimen coding 1 ~ 10) are shown in following table 11.
As known from Table 11, even if utilize the coarse crushing of mallet, also achieve the recovery of the level that can fully allow, also do not see the example showing low-down value, therefore can think, as long as there is the degree of fragmentation of this degree, then there is fully practical possibility.
Embodiment 6
By the coarse crushing of 38 brown rice samples, operate similarly to Example 1 subsequently with near infrared moisture meter (Co., Ltd. ケ Star ト scientific research is made, rice wheat moisture meter SP-1D3 type), make the extract of the inventive method.
On the other hand, from 38 identical brown rice samples, the extract of previous methods A is made similarly to Example 1 according to aforesaid previous methods A.
Then, to the extract made according to pre-treating method of the present invention and the extract made according to previous methods A, ICP-OES (SII VISTA-MPX) is used to measure the amount of cadmium, manganese, zinc, copper, lead, always each element of chromium, be used in the amount that the device (atom extinction photometer: Shimadzu Scisakusho Ltd AA-7000, hydride generation device: Shimadzu Scisakusho Ltd HVG-1) atom extinction photometer being attached with hydride generation device measures total arsenic.Then, the amount of the amount of mensuration element of the extract of method of the present invention and the mensuration element of the extract of previous methods A is compared, the ratio (%) of the amount of the mensuration element obtained with pre-treating method of the present invention relative to the amount of the mensuration element obtained with previous methods A is evaluated as the recovery.The value of this recovery more close to 100%, then represents that the extract obtained with pre-treating method of the present invention is more fully from plant cell structures extraction and determination element.Amount and the recovery of each mensuration element (cadmium, manganese, zinc, copper, lead, total chromium, total arsenic) obtained by use previous methods A and the pre-treating method of the present invention for each brown rice sample (specimen coding 1 ~ 38) are shown in following table 12.
As can be known from the results of Table 12, although the sample confirming to obtain with pre-treating method of the present invention can process at short notice, but in the same manner as the long previous methods A of needs, fully can extract the mensuration element of cadmium, manganese, zinc, copper, lead, chromium, arsenic.
Industry utilizes possibility
The pre-treatment of sample when pre-treating method of the present invention easily and at short notice can carry out the amount of the element measuring grain class, beans or plant cadmium, arsenic, zinc and/or manganese in the crop sample of subclass with high extraction ratio precision well, therefore, be very useful as the pre-treating method carried out near the scene.
Claims (7)
1. the pre-treating method of sample, it, for measuring the amount of at least one element in the group that is selected from and is made up of cadmium, arsenic, zinc, manganese, copper, lead and the chromium in the crop sample selected from grain class, beans or plant in subclass, is characterized in that, comprising:
The operation of (i) coarse crushing sample,
(ii) water be added into the sample through coarse crushing and heat, β starch transition contained in sample being become the operation of α starch,
(iii) enzyme is added into sample and is the operation of sugar by the α starch transition in sample,
(iv) hydrochloric acid be added into sample and extract the operation of the mensuration element in sample, and
V () removes the operation of solid from the liquid extracted.
2. the method for claim 1, is characterized in that, the coarse crushing of sample is the coarse crushing carried out when the moisture rate of sample measures.
3. method as claimed in claim 1 or 2, is characterized in that, utilize microwave to carry out the heating of the sample through coarse crushing.
4. the method as described in any one of claims 1 to 3, is characterized in that, uses diastase, proteinase and cellulase as enzyme.
5. the method as described in any one of Claims 1 to 4, is characterized in that, vibrate after adding enzyme to sample and after adding hydrochloric acid sample respectively.
6. the method as described in any one of Claims 1 to 5, is characterized in that, grain class is rice, wheat or buckwheat, and beans is soybean or peanut, and planting subclass is sesame or rapeseed.
7. tool box, is characterized in that, comprises the utensil for implementing the claims the method described in 1 ~ 6 any one and reagent.
Applications Claiming Priority (3)
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| JP2013109980 | 2013-05-24 | ||
| JP2013-109980 | 2013-05-24 | ||
| PCT/JP2014/063639 WO2014189123A1 (en) | 2013-05-24 | 2014-05-23 | Sample pre-treatment method for measuring the quantity of toxic elements in agricultural produce samples |
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| JP (1) | JP5666070B1 (en) |
| CN (1) | CN105452841A (en) |
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| CN109164220A (en) * | 2018-09-26 | 2019-01-08 | 贵州省三好食品开发有限公司 | Bean product raw material heavy metal content detection method |
| CN109507247A (en) * | 2018-12-11 | 2019-03-22 | 邯郸学院 | Identify the method in the millet place of production based on nonlinear chemical fingerprint |
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| JP2016057301A (en) * | 2014-09-08 | 2016-04-21 | 株式会社住化分析センター | Method for preparing sample for analysis of hazardous substance, kit for preparation, and method for analysis of hazardous substance |
| JP6764160B2 (en) * | 2016-09-24 | 2020-09-30 | 学校法人中部大学 | Preparation method of sample for hazard analysis |
| CN111579349A (en) * | 2020-06-09 | 2020-08-25 | 福建天甫电子材料有限公司 | Method for preparing ICP-MS sample by concentration |
| CN113866224B (en) * | 2021-12-01 | 2022-02-15 | 广东利诚检测技术有限公司 | Method for detecting content of harmful metal elements in food based on magnetoelectric coupling method |
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Also Published As
| Publication number | Publication date |
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| JPWO2014189123A1 (en) | 2017-02-23 |
| JP5666070B1 (en) | 2015-02-12 |
| WO2014189123A1 (en) | 2014-11-27 |
| HK1221284A1 (en) | 2017-05-26 |
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