CN114544306A - Detection method of heavy metals in rice - Google Patents
Detection method of heavy metals in rice Download PDFInfo
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- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 145
- 235000009566 rice Nutrition 0.000 title claims abstract description 145
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 78
- 238000001514 detection method Methods 0.000 title description 36
- 240000007594 Oryza sativa Species 0.000 title 1
- 241000209094 Oryza Species 0.000 claims abstract description 160
- 238000001035 drying Methods 0.000 claims abstract description 69
- 238000005406 washing Methods 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims description 180
- 230000029087 digestion Effects 0.000 claims description 148
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000007873 sieving Methods 0.000 claims description 10
- 210000005069 ears Anatomy 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims 2
- 238000010981 drying operation Methods 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000035800 maturation Effects 0.000 abstract description 11
- 238000011161 development Methods 0.000 abstract description 6
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 abstract description 6
- 230000008859 change Effects 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 20
- 239000000428 dust Substances 0.000 description 7
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- 238000004140 cleaning Methods 0.000 description 6
- 238000000120 microwave digestion Methods 0.000 description 6
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- 238000004458 analytical method Methods 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 235000019774 Rice Bran oil Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
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- 244000144972 livestock Species 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
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- 230000008569 process Effects 0.000 description 1
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- 239000008165 rice bran oil Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
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Abstract
The invention relates to a method for detecting heavy metals in rice, which comprises the following steps: the method comprises the steps of classifying and collecting rice in each period, respectively washing, drying, crushing and digesting the root in the elongation stage, the stem leaf in the elongation stage, the ear in the elongation stage, the root in the mature stage, the stem leaf in the mature stage and the seeds in the mature stage, and respectively measuring the total content of heavy metals by using an ICP-MS instrument to respectively digest the root in the elongation stage, the stem leaf in the maturation stage, the ear in the maturation stage, the root in the mature stage, the stem leaf in the mature stage and the seeds in the mature stage. The heavy metal pollution condition of the rice can be comprehensively detected and analyzed, the heavy metal pollution of the rice can be prevented and controlled in time, and the change condition and the trend of the heavy metal content of the rice along with growth and development can be analyzed and researched according to the condition of the heavy metal content of rice plants in different growth periods.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for detecting heavy metals in rice.
Background
The rice is annual aquatic herbage in the family of Gramineae, southern China is a main rice production area, northern provinces are planted, the rice is used as one of the most important grain crops in the world, more than half of the global population uses the rice as a main food source, the value of the rice is high, the rice can be used as staple food, rice bran is used as a rice cortex and can extract oil, rice bran oil is a whitening holy product, in addition, the rice bran can be used for pickling vegetables and even can be used as a single dish, namely fried rice bran, in addition, the rice bran is the rice hull and is an important source of animal feed, and the rice straw is another very special economic byproduct and can be eaten by cattle, sheep and other livestock, and in sum, the value of the rice is high and the application is very wide.
However, in recent years, environmental pollution is more and more serious and harmful to the health of people, heavy metal pollution is more and more concerned, rice is one of main grains of people, and the exceeding of the heavy metal content can directly affect the health of people, so that a comprehensive detection method for detecting the heavy metal content in the rice is needed to be provided for detecting the heavy metal content in the rice.
Disclosure of Invention
Based on this, it is necessary to provide a method for detecting heavy metals in rice.
A method for detecting heavy metals in rice comprises the following steps:
classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem and leaf in the jointing stage, respectively washing the root in the jointing stage and the stem and leaf in the jointing stage, drying to remove water, and respectively crushing the dried root in the jointing stage and the dried stem and leaf in the jointing stage to obtain root powder in the jointing stage and stem and leaf powder in the jointing stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and an ear in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage, drying to remove water, and respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and an ear powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, drying to remove water, and respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
respectively to the root powder of the jointing stage, the stem leaf powder of the jointing stage, the root powder of the booting stage, the stem leaf powder of the booting stage, the ear powder of the booting stage, the root powder of the maturing stage, the stem leaf powder of the maturing stage and the seed powder of the maturing stage, respectively carry out digestion treatment, and respectively carry out constant volume treatment to obtain the root digestion solution of the jointing stage, the stem leaf digestion solution of the jointing stage, the root digestion solution of the booting stage, the stem leaf digestion solution of the booting stage, the ear digestion solution of the booting stage, the root digestion solution of the maturing stage, the stem leaf digestion solution of the maturing stage and the seed digestion solution of the maturing stage, and respectively to the root digestion solution of the jointing stage, the stem leaf digestion solution of the jointing stage, the root digestion solution of the booting stage, the stem leaf digestion solution of the booting stage, the ear digestion solution of the booting stage, the stem leaf digestion solution of the booting stage, the head digestion solution of the booting stage, the stem leaf and the stem leaf, And determining the total content of heavy metals by using the root digestion solution in the mature period, the stem and leaf digestion solution in the mature period and the kernel digestion solution in the mature period.
In one embodiment, the drying temperature is controlled to be 58-62 ℃ in the operation of respectively washing the root in the jointing stage and the stem and leaf in the jointing stage and then drying.
In one embodiment, the drying temperature is controlled to be 58 to 62 ℃ in the operation of washing the root of the booting stage, the stem and leaf of the booting stage and the ear of the booting stage respectively and then drying the root, the stem and leaf of the booting stage and the ear of the booting stage.
In one embodiment, the drying temperature is controlled to be 58-62 ℃ in the operation of respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period and then drying.
In one embodiment, the acid solution is a nitric acid solution.
In one embodiment, the mass fraction of the nitric acid solution is 6% to 9%.
In one embodiment, the digestion is further performed by adding an acid solution to the root powder in the elongation stage, the stem and leaf powder in the elongation stage, the root powder in the booting stage, the stem and leaf powder in the booting stage, the ear powder in the booting stage, the root powder in the mature stage, the stem and leaf powder in the mature stage, and the seed powder in the mature stage, respectively.
In one embodiment, the dried root and stem leaves in the jointing stage are further subjected to a sieving operation after the crushing operation.
In one embodiment, after the crushing operation is performed on the dried root in the booting stage, the stem and leaf in the booting stage, and the ear in the booting stage, respectively, a sieving operation is further performed.
In one embodiment, after the crushing operation is performed on the dried root in the mature period, the stem and leaf in the mature period, and the kernel in the mature period, the sieving operation is further performed.
Compared with the prior art, the invention has at least the following advantages:
the method for detecting the heavy metal in the rice can obtain rice samples in each growth period by collecting the rice in different growth periods, then separate the rice samples in the jointing period, the rice samples in the booting period and the rice samples in the mature period, and respectively carry out cleaning, drying, crushing and digestion treatment, so that the heavy metal content of each part of the rice in different growth periods can be respectively measured and analyzed, thus, the heavy metal pollution condition of the rice can be comprehensively detected and analyzed, the heavy metal pollution of the rice can be timely prevented and controlled, the heavy metal pollution of the rice can be better treated and improved, the change condition and the trend of the heavy metal content of the rice along with the growth and development can be analyzed and researched according to the heavy metal content condition of the rice plants in different growth periods, can carry out comprehensive analysis on the heavy metal pollution of the rice more deeply and comprehensively, and has good practicability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a schematic flow chart of a method for detecting heavy metals in rice according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, in one embodiment, a method for detecting heavy metals in rice includes the following steps:
s110, classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage.
It should be noted that different growth periods of rice have different morphologies, growth, development and victory characteristics, specifically, the main growth period of rice is divided into a jointing stage, a booting stage and a mature stage, the jointing stage of rice is that the internode of the 5 th section from top to bottom of the rice plant begins to extend, at the same time, the scion of the rice plant begins to differentiate, at this time, the main morphology of the rice plant is divided into two parts of root and stem leaf, the booting stage of rice is that the scion of rice begins to differentiate, and develops to heading, at this time, the main morphology of the rice plant is divided into three parts of root, stem leaf and ear, the mature stage of rice is that the rice grain is mature, at this time, the main morphology of the rice plant is divided into root, stem leaf and seed, by classifying and collecting the rice in different growth periods, the rice sample in each growth period can be obtained, specifically, the jointing stage is divided into root, stem leaf and seed, The rice plants in the booting stage and the mature stage are collected and sampled, so that a rice sample in the jointing stage, a rice sample in the booting stage and a rice sample in the mature stage are obtained, and thus, the heavy metal content of the rice in different growth stages can be conveniently detected in the follow-up process, and the heavy metal pollution condition of the rice can be conveniently and comprehensively detected and analyzed.
S120, dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem leaf in the jointing stage, respectively washing the root in the jointing stage and the stem leaf in the jointing stage, then drying to remove water, and then respectively crushing the dried root in the jointing stage and the stem leaf in the jointing stage to obtain root powder in the jointing stage and stem leaf powder in the jointing stage.
It should be noted that, because the shape of the rice plant in the jointing stage mainly includes two parts of root and stem leaf, the root in the jointing stage and the stem leaf in the jointing stage are obtained by dividing the rice sample in the jointing stage into two parts of root and stem leaf, and then the two parts are washed respectively to remove the dirt on the root in the jointing stage and the stem leaf in the jointing stage, at this time, because the shape of the root and the stem leaf is different, the dirt condition is also different, for example, the root has soil, the stem leaf has dirt such as dust, etc., the root and the stem leaf in the jointing stage are washed respectively, the dirt can be washed more quickly and efficiently, the cleaning together is avoided, thereby the dirt is avoided, the cleaning is not convenient, after the washing, the clean root in the jointing stage and the stem leaf in the jointing stage can be obtained, thereby the normal operation of the subsequent heavy metal content detection is ensured, the damage to the instrument is avoided, and the detection result is not influenced, and then, respectively drying the washed root in the jointing stage and the stem and leaf in the jointing stage, removing water, drying the root in the jointing stage and the stem and leaf in the jointing stage, respectively obtaining root powder in the jointing stage and stem and leaf powder in the jointing stage by grinding into powder, and facilitating subsequent heavy metal content detection.
S130, dividing the rice sample in the booting period into three parts to obtain roots in the booting period, stems and leaves in the booting period and ears in the booting period, respectively washing the roots in the booting period, the stems and leaves in the booting period and the ears in the booting period, then drying the roots in the booting period, the stems and leaves in the booting period and the ears in the booting period to remove water, and then respectively crushing the dried roots in the booting period, the stems and leaves in the booting period and the ears in the booting period to obtain root powder in the booting period, stem and leaf powder in the booting period and ear powder in the booting period.
It should be noted that, because the morphology of the rice plant at the booting stage of the rice mainly comprises three parts of root, stem leaf and ear, the root, stem leaf and ear at the booting stage are obtained by dividing the rice sample at the booting stage into three parts of root, stem leaf and ear, and then the washing is respectively carried out to remove the dirt on the root, stem leaf and ear at the booting stage, at this time, because the morphology of root, stem leaf and ear is different, the dirt situation is also different, for example, the root has soil, the stem leaf and ear have dirt such as dust, the washing is carried out on the root, stem leaf and ear at the booting stage respectively, the dirt can be washed more quickly and efficiently, the washing together is avoided, thereby the soil and dust are prevented from mixing, the washing is inconvenient, after the washing is completed, the clean root, stem leaf and ear at the booting stage can be obtained, thereby ensuring the normal operation of the subsequent heavy metal content detection, avoiding the damage of soil and dust to the instrument, protecting the detection instrument and avoiding affecting the detection result, then respectively drying the washed root of the booting period, the stem leaf of the booting period and the ear of the booting period, removing water to dry the root of the booting period, the stem leaf of the booting period and the ear of the booting period, grinding into powder to respectively obtain the root powder of the booting period, the stem leaf powder of the booting period and the ear powder of the booting period, facilitating the subsequent heavy metal content detection, because the forms of the root, the stem leaf and the ear of the rice plant are greatly different and the water contents are different, respectively drying the washed root of the booting period, the stem leaf of the booting period and the ear of the booting period, facilitating the respective control of the drying temperature and time, avoiding the condition of over-drying or insufficient drying, therefore, the influence on the detection result can be avoided, the subsequent detection precision can be improved, and the accuracy of the detection result can be improved.
S140, dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, drying the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, removing water, and respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period.
It should be noted that, because the form of the rice plant in the mature period of the rice mainly comprises three parts of root, stem leaf and seed, the root in the mature period, the stem leaf in the mature period and the seed in the mature period are obtained by dividing the rice sample in the mature period into three parts of root, stem leaf and seed, and then are respectively washed to remove the dirt on the root in the mature period, the stem leaf in the mature period and the seed in the mature period, at this time, because the root has dirt such as soil, the stem leaf and the seed have dirt such as dust, and the dirt conditions of each part are different, the dirt can be washed more quickly and efficiently by respectively washing the root in the mature period, the stem leaf in the mature period and the seed in the mature period, so as to avoid the cleaning together, thereby avoiding the soil and dust mixing and affecting the cleaning efficiency, and the root in the mature period, the stem leaf in the mature period and the seed can be obtained cleanly after the washing, thereby ensuring the normal operation of the subsequent heavy metal content detection, avoiding soil and dust from damaging the instrument, protecting the detection instrument and influencing the detection result, then respectively drying the washed roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, removing water to dry the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, respectively obtaining the root powder in the mature period, the stem and leaf powder in the mature period and the seed powder in the mature period by grinding into powder, facilitating the subsequent heavy metal content detection, and avoiding the over-drying or insufficient drying condition by respectively drying the washed roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period due to the large shape difference and different water contents of rice plants, therefore, the influence on the detection result can be avoided, the subsequent detection precision can be improved, and the accuracy of the detection result can be improved.
S150, respectively to root powder in the jointing stage, stem leaf powder in the jointing stage, root powder in the booting stage, stem leaf powder in the booting stage, ear powder in the booting stage, root powder in the maturing stage, stem leaf powder in the maturing stage and acid liquor are added into the seed powder in the maturing stage to perform digestion treatment respectively and perform constant volume treatment respectively to obtain root digestion solution in the jointing stage, stem leaf digestion solution in the jointing stage, root digestion solution in the booting stage, stem leaf digestion solution in the booting stage, spike digestion solution in the booting stage, root digestion solution in the maturing stage, stem leaf digestion solution in the maturing stage and seed digestion solution in the maturing stage, and the root digestion solution in the jointing stage, the stem leaf digestion solution in the jointing stage, the root digestion solution in the booting stage, the stem leaf digestion solution in the booting stage, the spike digestion solution in the booting stage, the stem leaf digestion solution in the booting stage, the booting stage and the seed digestion solution in the booting stage, And determining the total content of heavy metals by using the root digestion solution in the mature period, the stem and leaf digestion solution in the mature period and the kernel digestion solution in the mature period.
It is to be noted that the root powder at the jointing stage, the stem and leaf powder at the jointing stage, the root powder at the booting stage, the stem and leaf powder at the booting stage, the ear powder at the booting stage, the root powder at the mature stage, the stem and leaf powder at the mature stage and the seed powder at the mature stage are respectively digested by a microwave digestion instrument, specifically, acid liquor is respectively added into the root powder at the jointing stage, the stem and leaf powder at the jointing stage, the root powder at the booting stage, the stem and leaf powder at the booting stage, the ear powder at the booting stage, the root powder at the mature stage, the stem and leaf powder at the mature stage and the seed powder at the mature stage, after standing for one day, the digestion is respectively carried out on the microwave digestion instrument, the first temperature rise is controlled to 120 ℃, the temperature rise time is 5min, the temperature rise time is controlled to 120 ℃, the second temperature rise is controlled to 150 ℃, the temperature rise time is 10min, the temperature rise is controlled to 150 ℃, the third temperature rise to 190 ℃, the temperature rise time is controlled to 5min, keeping the temperature at 190 ℃ for 20min to realize digestion treatment, thereby obtaining root digestion solution at the jointing stage, stem and leaf digestion solution at the jointing stage, root digestion solution at the booting stage, stem and leaf digestion solution at the booting stage, ear digestion solution at the booting stage, root digestion solution at the mature stage, stem and leaf digestion solution at the mature stage and seed digestion solution at the mature stage to be detected respectively by an ICP-MS instrument, the root digestion solution at the jointing stage, the stem and leaf digestion solution at the jointing stage, the root digestion solution at the booting stage, the stem and leaf digestion solution at the booting stage, the ear digestion solution at the booting stage, the root digestion solution at the mature stage, the stem and leaf digestion solution at the mature stage and the seed digestion solution at the mature stage, thus, the heavy metal content conditions of different parts of the rice at each stage can be obtained, thus, the heavy metal pollution conditions of the rice can be detected and analyzed comprehensively, and the heavy metal pollution of the rice can be prevented and treated in time, therefore, the heavy metal pollution of the rice can be better treated and improved, the change condition and the trend of the heavy metal content of the rice along with growth and development can be analyzed and researched according to the conditions of the heavy metal content of rice plants in different growth periods, the heavy metal pollution of the rice can be more deeply and comprehensively analyzed, and the practicability is good.
In one embodiment, the drying temperature is controlled to be 58-62 ℃ in the operation of respectively washing the root in the jointing stage and the stem and leaf in the jointing stage and then drying. It can be understood that the drying temperature is controlled to be 58-62 ℃, the drying temperature is moderate, the phenomenon that the root of the jointing stage and the stem leaves of the jointing stage are burnt and damaged due to overhigh temperature is avoided, meanwhile, the phenomenon that the drying temperature is too low to influence the drying efficiency is avoided, and therefore, the root of the jointing stage and the stem leaves of the jointing stage can be better and faster dried.
In one embodiment, the drying temperature is controlled to be 58 to 62 ℃ in the operation of washing the root of the booting stage, the stem and leaf of the booting stage and the ear of the booting stage respectively and then drying the root, the stem and leaf of the booting stage and the ear of the booting stage. It can be understood that the drying temperature is controlled to be 58-62 ℃, the drying temperature is moderate, the phenomenon that the temperature is too high and the root of the booting stage, the stem leaf of the booting stage and the ear of the booting stage are burnt and damaged is avoided, meanwhile, the phenomenon that the drying temperature is too low and the drying efficiency is influenced is avoided, and therefore the root of the booting stage, the stem leaf of the booting stage and the ear of the booting stage can be better and faster dried.
In one embodiment, the drying temperature is controlled to be 58-62 ℃ in the operation of respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period and then drying. It can be understood that by controlling the drying temperature to be 58-62 ℃, the drying temperature can be ensured to be moderate, the phenomenon that the temperature is too high to burn and damage roots in the mature period, stems and leaves in the mature period and seeds in the mature period can be avoided, and meanwhile, the phenomenon that the drying efficiency is influenced by too low drying temperature can be avoided, so that the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period can be ensured to be dried better and faster.
In one embodiment, the acid solution is a nitric acid solution. The mass fraction of the nitric acid solution is 6-9%. It can be understood that in this embodiment, the acid solution for digestion treatment is a nitric acid solution with a mass fraction of 6% to 9%, which can ensure normal operation of digestion operation, and the nitric acid solution has a moderate concentration and avoids an excessively high concentration, thereby greatly improving the safety of digestion operation, and the acid content in the extracted root digestion solution, the extracted stem and leaf digestion solution, the pregnant root digestion solution, the pregnant stem and leaf digestion solution, the pregnant ear digestion solution, the mature root digestion solution, the mature stem and leaf digestion solution and the mature seed digestion solution obtained after digestion is lower, thereby greatly reducing the subsequent damage degree to the detection instrument, and being beneficial to improving the service life of the detection instrument.
In one embodiment, the digestion is further performed by adding an acid solution to the root powder in the elongation stage, the stem and leaf powder in the elongation stage, the root powder in the booting stage, the stem and leaf powder in the booting stage, the ear powder in the booting stage, the root powder in the mature stage, the stem and leaf powder in the mature stage, and the seed powder in the mature stage, respectively. It can be understood that the prepared root digestion solution in the elongation stage, the stem and leaf digestion solution in the elongation stage, the root digestion solution in the booting stage, the stem and leaf digestion solution in the booting stage, the spike digestion solution in the booting stage, the root digestion solution in the maturation stage, the stem and leaf digestion solution in the maturation stage and the kernel digestion solution in the maturation stage can be further reduced in time by performing acid dispelling operation in time after digestion treatment, so that a detection instrument can be further protected, and normal subsequent detection can be ensured. Specifically, in the above-mentioned operations of separately performing the acid-removing operation, the acid-removing temperature is controlled to 85 to 95 ℃ and the acid-removing time is controlled to 4 to 5 hours under vacuum conditions. In this way, under the vacuum condition, the promotion of the acid-dispelling operation is facilitated, the efficiency of the acid-dispelling operation is ensured, in addition, as the higher the temperature is, the promotion of the molecular motion is facilitated, so that the nitric acid molecules in the solution system can be volatilized out of the solution system more quickly, but as the rice is a plant sample, the components of each part in each period are more complex, and the deterioration is easy to occur when the rice is heated at the high temperature for a long time, the acid-dispelling treatment is carried out under the vacuum condition, the acid-dispelling temperature is set to be 85-95 ℃, the acid-dispelling temperature is moderate, the influence of the long-time high-temperature treatment on the properties of the root powder in the jointing stage, the stem leaf powder in the jointing stage, the root powder in the pregnancy stage, the stem leaf powder in the pregnancy stage, the ear powder in the pregnancy stage, the root powder in the maturation stage, the powder in the maturation stage and the kernel powder in the maturation stage in the solution system can be avoided, therefore, the acid content is reduced, damage to an instrument is avoided, accuracy and precision of heavy metal detection are guaranteed, and a detection result is guaranteed.
In one embodiment, the dried root and stem leaves in the jointing stage are further subjected to a sieving operation after the crushing operation. It can be understood that, through the operation of sieving, can obtain the root powder of the even jointing stage of granule and the stem leaf powder of jointing stage, avoid having the root powder of the jointing stage of large granule and the stem leaf powder of jointing stage, avoid subsequent detection time measuring to cause the damage to detecting instrument to be favorable to guaranteeing the normal clear of detection, guarantee to detect the accuracy.
In one embodiment, after the crushing operation is performed on the dried root in the booting stage, the stem and leaf in the booting stage, and the ear in the booting stage, respectively, a sieving operation is further performed. It can be understood that, through sieving the operation, can obtain the root powder of the even root powder of pulling out pregnant fringe period of granule, the stem leaf powder of pregnant fringe period and the ear of grain powder of pregnant fringe period, avoid having the root powder of pregnant fringe period of large granule, the stem leaf powder of pregnant fringe period and the ear of grain powder of pregnant fringe period, avoid follow-up detection time measuring to cause the damage to detecting instrument to be favorable to guaranteeing the normal clear of detection, guarantee to detect the accuracy.
In one embodiment, after the crushing operation is performed on the dried root in the mature period, the stem and leaf in the mature period, and the kernel in the mature period, the sieving operation is further performed. It can be understood that the root powder in the mature period, the stem and leaf powder in the mature period and the seed powder in the mature period can be obtained by sieving, the existence of large particles of the root powder in the mature period, the stem and leaf powder in the mature period and the seed powder in the mature period is avoided, and the damage to a detection instrument during subsequent detection is avoided, so that the normal detection can be ensured, and the detection accuracy can be ensured.
Compared with the prior art, the invention has at least the following advantages:
the method for detecting the heavy metal in the rice can obtain rice samples in each growth period by collecting the rice in different growth periods, then separate the rice samples in the jointing period, the rice samples in the booting period and the rice samples in the mature period, and respectively carry out cleaning, drying, crushing and digestion treatment, so that the heavy metal content of each part of the rice in different growth periods can be respectively measured and analyzed, thus, the heavy metal pollution condition of the rice can be comprehensively detected and analyzed, the heavy metal pollution of the rice can be timely prevented and controlled, the heavy metal pollution of the rice can be better treated and improved, the change condition and the trend of the heavy metal content of the rice along with the growth and development can be analyzed and researched according to the heavy metal content condition of the rice plants in different growth periods, can carry out comprehensive analysis on the heavy metal pollution of the rice more deeply and comprehensively, and has good practicability.
The following are detailed description of the embodiments
Example 1
Classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem and leaf in the jointing stage, respectively washing the root in the jointing stage and the stem and leaf in the jointing stage, then drying at 58 ℃ to remove water, and then respectively crushing the dried root in the jointing stage and the dried stem and leaf in the jointing stage to obtain root powder in the jointing stage and stem and leaf powder in the jointing stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and an ear in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage, then drying at 58 ℃ to remove water, and then respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and an ear powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, then drying at the drying temperature of 58 ℃ to remove water, and then respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
respectively adding 18mL of nitric acid solution with the mass fraction of 6% into 1g of root powder of the jointing stage, 1g of stem and leaf powder of the jointing stage, 1g of ear powder of the jointing stage, 1g of root powder of the maturing stage, 1g of stem and leaf powder of the maturing stage and 1g of seed powder of the maturing stage, standing for one day, respectively performing digestion treatment on a microwave digestion instrument, controlling the temperature to rise to 120 ℃ for the first time, the temperature to rise to 5min for the second time, the temperature to rise to 150 ℃ for 10min for the second time, the temperature to rise to 10min for the third time, the temperature to 190 ℃ for the third time, the temperature to rise to 5min for 190 ℃ for 20min, and respectively performing constant volume treatment to obtain root digestion solution of the jointing stage, stem and leaf digestion solution of the jointing stage, root digestion solution of the jointing stage, stem and leaf digestion solution of the jointing stage, and leaf digestion solution of the jointing stage, The method comprises the following steps of respectively determining the total content of heavy metals by using a spike digestion liquid in a booting stage, a root digestion liquid in a mature stage, a stem leaf digestion liquid in the mature stage and a kernel digestion liquid in the mature stage, and then respectively determining the total content of the heavy metals by using an ICP-MS instrument.
Example 2
Classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem and leaf in the jointing stage, respectively washing the root in the jointing stage and the stem and leaf in the jointing stage, then drying at 60 ℃ to remove water, and then respectively crushing the dried root in the jointing stage and the dried stem and leaf in the jointing stage to obtain root powder in the jointing stage and stem and leaf powder in the jointing stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and a spike in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the spike in the booting stage, then drying at 60 ℃ to remove water, and then respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the spike in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and a spike powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, then drying at the drying temperature of 60 ℃ to remove water, and then respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
respectively adding 18mL of nitric acid solution with the mass fraction of 8% into 1g of root powder of the jointing stage, 1g of stem and leaf powder of the jointing stage, 1g of ear powder of the jointing stage, 1g of root powder of the maturing stage, 1g of stem and leaf powder of the maturing stage and 1g of seed powder of the maturing stage, standing for one day, performing digestion treatment on a microwave digestion instrument respectively, controlling the temperature to rise to 120 ℃ for the first time, the temperature to rise to 5min for 120 ℃, the temperature to rise to 150 ℃ for the second time, the temperature to rise to 10min for 150 ℃, the temperature to rise to 190 ℃ for the third time, the temperature to rise to 5min, the temperature to rise to 190 ℃ for 20min, and performing constant volume treatment respectively to obtain root digestion solution of the jointing stage, stem and leaf digestion solution of the jointing stage, root digestion solution of the jointing stage, stem and leaf digestion solution of the jointing stage, and leaf digestion solution of the jointing stage, The method comprises the following steps of respectively determining the total content of heavy metals by using a spike digestion liquid in a booting stage, a root digestion liquid in a mature stage, a stem leaf digestion liquid in the mature stage and a kernel digestion liquid in the mature stage, and then respectively determining the total content of the heavy metals by using an ICP-MS instrument.
Example 3
Classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem and leaf in the jointing stage, respectively washing the root in the jointing stage and the stem and leaf in the jointing stage, then drying at 62 ℃ to remove water, and then respectively crushing the dried root in the jointing stage and the dried stem and leaf in the jointing stage to obtain root powder in the jointing stage and stem and leaf powder in the jointing stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and an ear in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage, then drying at 62 ℃ to remove water, and then respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and an ear powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, then drying at the drying temperature of 62 ℃ to remove water, and then respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
respectively adding 18mL of nitric acid solution with the mass fraction of 9% into 1g of root powder of the jointing stage, 1g of stem and leaf powder of the jointing stage, 1g of ear powder of the jointing stage, 1g of root powder of the maturing stage, 1g of stem and leaf powder of the maturing stage and 1g of seed powder of the maturing stage, standing for one day, performing digestion treatment on a microwave digestion instrument, controlling the temperature to rise to 120 ℃ for the first time, the temperature to rise to 5min for 120 ℃, the temperature to rise to 150 ℃ for the second time, the temperature to rise to 10min for 150 ℃, the temperature to rise to 190 ℃ for the third time, the temperature to rise to 5min, the temperature to rise to 190 ℃ for 20min, and performing constant volume treatment to obtain root digestion solution of the jointing stage, stem and leaf digestion solution of the jointing stage, and leaf digestion solution of the jointing stage, The method comprises the following steps of respectively determining the total content of heavy metals by using a spike digestion liquid in a booting stage, a root digestion liquid in a mature stage, a stem leaf digestion liquid in the mature stage and a kernel digestion liquid in the mature stage, and then respectively determining the total content of the heavy metals by using an ICP-MS instrument.
Example 4
Classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the elongation stage into two parts to obtain a root in the elongation stage and a stem and leaf in the elongation stage, respectively washing the root in the elongation stage and the stem and leaf in the elongation stage, then drying at the drying temperature of 60 ℃ to remove water, and then respectively crushing the dried root in the elongation stage and the stem and leaf in the elongation stage to obtain root powder in the elongation stage and stem and leaf powder in the elongation stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and a spike in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the spike in the booting stage, then drying at 60 ℃ to remove water, and then respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the spike in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and a spike powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, then drying at the drying temperature of 60 ℃ to remove water, and then respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
adding 18mL of nitric acid solution with the mass fraction of 8% into 1g of root powder in the jointing stage, 1g of stem and leaf powder in the jointing stage, 1g of ear powder in the jointing stage, 1g of root powder in the mature stage, 1g of stem and leaf powder in the mature stage and 1g of seed powder in the mature stage respectively, standing for one day, performing digestion treatment on a microwave digestion instrument respectively, controlling the temperature to rise to 120 ℃ for the first time, the temperature to rise to 5min at 120 ℃, the temperature to rise to 120 ℃ for 5min at 120 ℃, the temperature to rise to 150 ℃ for the second time, the temperature to rise to 10min at 150 ℃, the temperature to rise to 190 ℃ for the third time, the temperature to rise to 5min at 190 ℃, the temperature to rise to 20min at 190 ℃, performing acid removal operation respectively, controlling the acid removal temperature to 92 ℃ and the acid removal time to 5h under the vacuum condition, and performing volume fixing treatment respectively, obtaining root digestion solution at the jointing stage, stem leaf digestion solution at the jointing stage, root digestion solution at the booting stage, stem leaf digestion solution at the booting stage, ear digestion solution at the booting stage, root digestion solution at the maturing stage, stem leaf digestion solution at the maturing stage and kernel digestion solution at the maturing stage, and respectively determining the total content of heavy metals by using an ICP-MS instrument through the root digestion solution at the jointing stage, the stem leaf digestion solution at the jointing stage, the root digestion solution at the booting stage, the stem leaf digestion solution at the booting stage, the ear digestion solution at the booting stage, the root digestion solution at the maturing stage, the stem leaf digestion solution at the maturing stage and the kernel digestion solution at the maturing stage.
Performance evaluation: to the root-digested liquid at the elongation stage, the stem-and-leaf-digested liquid at the elongation stage, the root-digested liquid at the booting stage, the stem-and-leaf-digested liquid at the booting stage, the ear-digested liquid at the booting stage, the root-digested liquid at the maturation stage, the stem-and-leaf-digested liquid at the maturation stage, and the kernel-digested liquid at the maturation stage of examples 2 and 4, 5mg/L of a cadmium heavy metal solution was added, the cadmium heavy metal concentrations before and after the labeling were measured, and the recovery rates were calculated, specifically, the recovery rates were (concentration after the labeling-concentration before the labeling)/concentration of the labeling amount × 100%, and the results are shown in table 1.
As can be seen from Table 1, the method for testing heavy metals in rice provided by the invention has the advantages that the recovery rate of the measured numerical value is good, the detection precision is high, the heavy metal content of each part of the rice in different growth periods can be respectively measured and analyzed, so that the heavy metal pollution condition of the rice can be comprehensively detected and analyzed, the heavy metal pollution of the rice can be timely prevented and controlled, the heavy metal pollution of the rice can be better treated and improved, the change condition and trend of the heavy metal content of the rice along with growth and development can be analyzed and researched according to the heavy metal content condition of rice plants in different growth periods, the heavy metal pollution of the rice can be comprehensively analyzed more deeply, and the practicability is good.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for detecting heavy metals in rice is characterized by comprising the following steps:
classifying and collecting the rice in each period to obtain a rice sample in an elongation stage, a rice sample in a booting stage and a rice sample in a mature stage;
dividing the rice sample in the jointing stage into two parts to obtain a root in the jointing stage and a stem and leaf in the jointing stage, respectively washing the root in the jointing stage and the stem and leaf in the jointing stage, drying to remove water, and respectively crushing the dried root in the jointing stage and the dried stem and leaf in the jointing stage to obtain root powder in the jointing stage and stem and leaf powder in the jointing stage;
dividing the rice sample in the booting stage into three parts to obtain a root in the booting stage, a stem leaf in the booting stage and an ear in the booting stage, respectively washing the root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage, drying to remove water, and respectively crushing the dried root in the booting stage, the stem leaf in the booting stage and the ear in the booting stage to obtain a root powder in the booting stage, a stem leaf powder in the booting stage and an ear powder in the booting stage;
dividing the rice sample in the mature period into three parts to obtain roots in the mature period, stems and leaves in the mature period and seeds in the mature period, respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period, drying to remove water, and respectively crushing the dried roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period to obtain root powder in the mature period, stem and leaf powder in the mature period and seed powder in the mature period;
respectively adding acid liquor into the root powder in the elongation stage, the stem leaf powder in the elongation stage, the root powder in the booting stage, the stem leaf powder in the booting stage, the spike powder in the booting stage, the root powder in the mature stage, the stem leaf powder in the mature stage and the seed powder in the mature stage, respectively digesting, respectively performing constant volume treatment to obtain the root digestion liquor in the elongation stage, the stem leaf digestion liquor in the elongation stage, the root digestion liquor in the booting stage, the stem leaf digestion liquor in the booting stage, the spike digestion liquor in the booting stage, the root digestion liquor in the mature stage, the stem leaf digestion liquor in the mature stage and the seed digestion liquor in the mature stage, and respectively subjecting the root digestion liquor in the elongation stage, the stem leaf digestion liquor in the elongation stage, the root digestion liquor in the booting stage, the stem leaf digestion liquor in the booting stage, the spike digestion liquor in the booting stage, the stem leaf digestion liquor in the booting stage, the spike digestion liquor in the booting stage, the spike digestion liquor in the spike stage, the booting stage, the stem leaf, the seed, the stem leaf, the stem and leaf, the stem leaf digestion liquor in the stem and leaf, the stem digestion liquor in the stem, the stem and leaf, the stem, the, And determining the total content of heavy metals by using the root digestion solution in the mature period, the stem and leaf digestion solution in the mature period and the kernel digestion solution in the mature period.
2. The method for detecting heavy metals in rice as claimed in claim 1, wherein the drying temperature is controlled to be 58 ℃ to 62 ℃ in the washing operation and the drying operation of the roots in the jointing stage and the stems and leaves in the jointing stage, respectively.
3. The method for detecting heavy metals in rice as claimed in claim 1, wherein the drying temperature is controlled to be 58 ℃ to 62 ℃ in the operations of washing the roots in the booting stage, the stems and leaves in the booting stage, and the ears in the booting stage, respectively, and then drying the washed roots, the stems and leaves in the booting stage, and the ears in the booting stage.
4. The method for detecting the heavy metals in the rice as claimed in claim 1, wherein the drying temperature is controlled to be 58-62 ℃ in the operation of respectively washing the roots in the mature period, the stems and leaves in the mature period and the seeds in the mature period and then drying the roots, the stems and leaves in the mature period and the seeds in the mature period.
5. The method for detecting the heavy metal in the rice as claimed in claim 1, wherein the acid solution is a nitric acid solution.
6. The method for detecting the heavy metal in the rice according to claim 5, wherein the mass fraction of the nitric acid solution is 6-9%.
7. The method according to claim 1, wherein an acid solution is added to the root powder in the elongation stage, the stem and leaf powder in the elongation stage, the root powder in the booting stage, the stem and leaf powder in the booting stage, the ear powder in the booting stage, the root powder in the mature stage, the stem and leaf powder in the mature stage, and the seed powder in the mature stage, respectively, and digestion is performed, and then acid-removing operation is performed.
8. The method for detecting heavy metals in rice as claimed in claim 1, wherein the screening operation is further performed after the crushing operation is performed on the dried root in the jointing stage and the dried stem and leaf in the jointing stage, respectively.
9. The method for detecting heavy metals in rice as claimed in claim 1, wherein a sieving operation is further performed after the operation of pulverizing the dried roots of the booting stage, the stems and leaves of the booting stage, and the ears of the booting stage, respectively.
10. The method for detecting heavy metals in rice as claimed in claim 1, wherein the screening operation is further performed after the crushing operation is performed on the dried roots in the mature period, the stems and leaves in the mature period, and the seeds in the mature period, respectively.
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