CN110411805A - Extracting method, extraction element and its application of mercury shape in a kind of cereal - Google Patents
Extracting method, extraction element and its application of mercury shape in a kind of cereal Download PDFInfo
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- CN110411805A CN110411805A CN201910844479.XA CN201910844479A CN110411805A CN 110411805 A CN110411805 A CN 110411805A CN 201910844479 A CN201910844479 A CN 201910844479A CN 110411805 A CN110411805 A CN 110411805A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention provides extracting method, extraction element and its applications of mercury shape in a kind of cereal, and described method includes following steps: grain sample and L-cysteine solution being mixed, mercury shape is extracted after ultrasonication, insoluble substance is removed, takes supernatant to be measured.The extracting method of mercury shape is fast and convenient in cereal of the present invention, and extracting solution can measure total mercury and inorganic mercury, methyl mercury and other mercury shapes simultaneously；Sample is not necessarily to soaked overnight, does not use acid-base reagent, catches up with acid or adjusting extracting liquid pH value without heating before upper machine testing, extractant is L-cysteine, it is non-hazardous to human body and environment, it is the mercury shape mercury in extractable sample using ultrasonication 5min, recovery rate is up to 95% or more.
Description
Technical field
The present invention relates to Chemical Decomposition field, it is related to the extracting method of mercury shape, extraction element in a kind of cereal and its answers
With.
Background technique
Main grain will include paddy, wheat, corn and beans etc., and grain and its product are the most basic diet groups of the mankind
At, wherein the not only mineral nutrient element indispensable containing human bodies such as magnesium, potassium and calcium, but also have containing lead, cadmium and mercury etc. to human body
Harmful heavy metal element.Wherein the common natural form of mercury element includes inorganic mercury and organic mercury (methyl mercury, ethyl mercury and phenyl
Mercury), methyl mercury is one of strongest mercury compound of toxicity, it has lipophilicity, can enter people by the enrichment of food chain
Body seriously threatens human health.Therefore comprehensively the content of analysis grain and its product Mineral Elements and heavy metal element, form and
Distribution understands grain nutrition to resident and safety is of great significance.
In grain and its product mercury element total amount detect traditional pre-treating method include High Pressure Digestion, micro-wave digestion and
The methods of reflux resolution, these method and steps are cumbersome, and time-consuming, it usually needs 2~6h, most methods need sample to impregnate
At night, strong corrosive acid and oxidising agent usage amount are big, need hot conditions and particular instrument, heating is also needed to catch up with acid after the completion of resolution
Or ultrasonic degassing, the security risk of operator is also increased while increasing sample to be tested loss and contaminated risk；Separately
Outer mercury is Low-Temperature Element, the degassing link before constant volume, as temperature control shakiness will lead to the evolution of mercury.The biography of mercury shape detection
System pre-treating method is ultrasonic water bath extraction method, and Extractant concentration is 5mol/L hydrochloric acid, and sample overnight uses ultrasonic water after impregnating
1h is extracted in bath, during which also needs shaking for several times, and for the pH environment (pH is 2~7) for taking into account reverse-phase chromatographic column tolerance, extracting solution is in upper machine
It needs frequently to adjust solution ph before detection, this process misoperation easily causes the loss of inorganic mercury, leads to inorganic mercury and methyl
The adduction data of mercury are lower than Determination of Total Mercury result.It can be seen that time-consuming for conventional mercury element and the pretreatment process of form, operation
It is cumbersome, a large amount of soda acids and oxidising agent are consumed in experiment, it is difficult to adapt to the demand that the high-throughput green of gross sample quickly detects.
Ultrasonic extraction is that cavitation effect, mechanical oscillation and disturbance effect generated using Ultrasonic Radiation pressure etc. is more
Grade effect, increases the motion frequency and speed of material molecule, increases solvent penetration power, so that target component be accelerated to enter solvent
A kind of extracting method.Conventional ultrasound immersion method extracts the mercury shape in grain and its product, and common instrument is ultrasonic cleaning machine, should
Instrument power is lower to cause extraction time too long, and generation noise is larger in the process of running, and long-time operation will affect experiment people
Member's health.In addition, China's current standard system or other documents are still in space state to the extracting method of inorganic mercury in sample.
CN103575583A discloses one kind and quickly mildly extracts heavy metal method from cereal, the steps include: cereal
Sample comminution is mixed with diluted acid, extracts heavy metal ion；By carrying out standing or centrifugal treating, grain sample after shaking, being vortexed
In the heavy metal elements such as cadmium, lead and mercury be transferred in supernatant substantially, the supernatant of acquisition is for detecting.But before this method
The processing time is still longer, need to extract 30min, preferably 10~15min, and the sample that processing obtains according to the different longests of element
Liquid is not used to the detection of mercury shape, and in addition diluted acid used still has certain harm to human body and environment.
Therefore it provides a kind of, quickly, in the extraction cereal of environmental protection the method for mercury shape is of great significance.
Summary of the invention
In view of the deficiencies of the prior art and actual demand, the present invention provide the extracting method of mercury shape in a kind of cereal,
Extraction element and its application, the present invention replace acid or lye commonly used in the prior art to extract grain sample using L-cysteine
In mercury shape, extracting solution can directly measure the variforms mercury such as total mercury and inorganic mercury, methyl mercury and ethyl mercury, while this method
Extraction time is short, and L-cysteine is non-toxic and tasteless, very friendly to experimenter and environment.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, described method includes following steps the present invention provides a kind of extracting method of mercury shape in cereal:
Grain sample and L-cysteine solution are mixed, mercury shape is extracted after ultrasonication, insoluble substance is removed, takes
Supernatant is to be measured.
The present invention replaces acid solution using L-cysteine, can effectively extract mercury shape in cereal, extracting solution is not necessarily to
Heating is carried out to catch up with acid or adjust pH value, it can when being used directly for subsequent detection, while avoiding current method processing inorganic mercury
Can there are problems that loss, a variety of mercury shapes in more accurate complete detection cereal ensure food safety.
Preferably, the method also includes pre-treatment steps: grain sample is crushed.
Preferably, the smashed partial size of the grain sample be less than 0.5mm, such as can be 0.1mm, 0.2mm, 0.3mm,
0.4mm or 0.5mm, preferably 0.2~0.3mm.
Preferably, the mass fraction of the L-cysteine is 0.05~0.5%, for example, can be 0.05%, 0.1%,
0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, preferably 0.1~0.2%.
In the present invention, in the range of the mass fraction of L-cysteine is 0.05~0.5%, nothing before upper machine testing total mercury
It need to heat and catch up with acid or degassing, be not necessarily to adjust pH before detecting mercury shape, obtained extracting solution is used directly for detecting, quick ring
It protects, simplifies the pre-treatment step of mercury shape in grain sample, shorten extraction time.
Preferably, the volume mass ratio of the L-cysteine solution and grain sample is greater than 10:1.
In the present invention, the volume mass of L-cysteine solution and grain sample ratio is set greater than 10:1, can be made
Different mercury shapes leachings are more complete, and ratio is less than 10:1 and is unfavorable for subsequent detection.
Preferably, the instrument of the ultrasound is ultrasonic cell disruption instrument.
Ultrasonic cleaner is generallyd use in the prior art and carries out mercury shape extraction, but before use instrument extraction, sample is needed
Carry out stay overnight immersion and etc., the time is long, and noise is big, and the present invention use ultrasonic cell disruption instrument, power is big, can be effective
The sound proof box for reducing extraction time, and being equipped with can reduce the noise of the sending in extraction process.
Preferably, the power of the ultrasound be 100~150W, such as can be 100W, 110W, 120W, 130W, 140W or
150W。
The present invention utilizes ultrasonication technology, selects non-toxic and tasteless L-Cys solution as single extractant, establishes one kind
Quickly mercury element and form extracting method in the cereal of environmental protection, low concentration L-cysteine solution cooperates the ultrasound of low-power, short
It can extract a variety of mercury shapes in time；For total mercury, without deaerating or catching up with acid after being extracted using this method；For mercury shape,
The pH value of low concentration L-cysteine solution meets the tolerance range of reverse-phase chromatographic column, is not necessarily to adjust extracting solution before examination with computer
PH effectively avoids mercury element from losing and reduces sample pollution risk；And after the pretreatment process of total mercury and mercury shape can save
Continuous constant volume link, it is quick that the operation is more convenient.
Preferably, the mode of the ultrasound is interval ultrasound, and ultrasonic 10s stops 1~5s.
Preferably, the time of the ultrasound is 3~5min, such as can be 3min, 4min or 5min.
The present invention completes to extract in 5min, extracting solution can by optimizing Extractant concentration and ultrasonication parameter
A variety of mercury shapes such as total mercury and inorganic mercury, methyl mercury and ethyl mercury are measured simultaneously, and L-cysteine is low as extractant price
Honest and clean, for 25g specification price less than 50 yuan, method is simple and efficient to handle.
Preferably, the mercury shape includes inorganic mercury, methyl mercury and ethyl mercury.
Preferably, the method for the removal insoluble substance includes standing, be centrifuged or filtering.
Preferably, the revolving speed of the centrifugation be 4000~20000rpm, such as can be 4000rpm, 5000rpm,
6000rpm、7000rpm、8000rpm、9000rpm、10000rpm、12000rpm、14000rpm、15000rpm、18000rpm
Or 20000rpm.
Preferably, the time of the centrifugation be 2~15min, such as can be 2min, 3min, 4min, 5min, 6min,
7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min or 15min.
Preferably, the filter membrane being filtered into using aperture less than 0.45 μm is filtered, such as can be 0.1 μm, 0.2
μm, 0.3 μm, 0.4 μm or 0.45 μm, preferably 0.2~0.3 μm.
Preferably, the step of the method also includes detection total mercury and mercury shapes.
The extracting solution that the present invention obtains is directly used in subsequent mercury shape detection, on chromatographic column and detecting instrument without influence, mentions
High detection efficiency.
In the present invention, the detection method of the total mercury can be atomic absorption spectrography (AAS), atomic fluorescence spectrometry, inductance coupling
Close Plasma Mass Spectrometry, inductively coupled plasma emission spectrography, spectrophotometer method or electrochemical workstation method；
The detection method of the mercury shape can be liquid chromatogram-inductivity coupled plasma mass spectrometry combination method or liquid phase color
Spectrum-atomic fluorescence spectrophotometry is combined method.
Second aspect, the present invention provide a kind of extraction element of mercury shape in cereal, and the extraction element uses such as first
Method described in aspect extracts mercury shape from cereal, and the extraction element includes driving unit 1, ultrasound unit 2, electronic control unit
3 and display unit 4；
The driving unit 1 is connected by transmission device with ultrasound unit 2, the driving unit 1, ultrasound unit 2, display
Unit 4 is connect with electronic control unit 3 respectively；
The driving unit includes drive shaft 11 and motor 12, and the drive shaft 11 is connected directly with motor 12；
The ultrasound unit includes ultrasonic head 21, pan straddle 7, and the ultrasound head 21 includes ultrasonic amplitude transformer 211.
Extraction element of the invention is a kind of quick pretreatment equipment that heavy metal in cereal is extracted using ultrasonication, is fitted
For heavy metal element in grain sample and the pre-treatment link of form on-site test.
Preferably, a length of 30~50cm of the extraction element, width are 20~40cm, and a height of 30~50cm, the length can
Be 30cm, 31cm, 32cm, 33cm, 34cm, 35cm, 36cm, 37cm, 38cm, 39cm, 40cm, 41cm, 42cm, 43cm,
44cm, 45cm, 46cm, 47cm, 48cm, 49cm or 50cm, the width can for 20cm, 21cm, 22cm, 23cm, 24cm,
25cm, 26cm, 27cm, 28cm, 29cm, 30cm, 31cm, 32cm, 33cm, 34cm, 35cm, 36cm, 37cm, 38cm, 39cm or
40cm, the height can be 30cm, 31cm, 32cm, 33cm, 34cm, 35cm, 36cm, 37cm, 38cm, 39cm, 40cm, 41cm,
The size of 42cm, 43cm, 44cm, 45cm, 46cm, 47cm, 48cm, 49cm or 50cm, described device can be in the ranges
Appropriate adjustment meets the function of corresponding units, preferably long 32cm, wide 25cm, high 30cm.
Preferably, the transmission device is belt 5.
In the present invention, transmission device is used to adjust the position of sample container, by adjusting appearance in a certain specific embodiment
The position of device bracket, rises sample container, is fixed on the ultrasonic amplitude transformer on ultrasonic head and immerses in sample extracting solution, completes to mention
Take process.
Preferably, the pan straddle 7 is connected with liquid level sensor 6.
In the present invention, liquid level sensor, the depth of detection probe immersed in liquid level, the phase of accurate control probe and liquid level are set
To position, keep ultrasonic procedure more fast and effective.
Preferably, the sample container includes centrifuge tube 22, and the specification of the centrifuge tube 22 is 10mL or 15mL.
In the present invention, the container of grain sample and L-cysteine solution is placed in design, and places the bracket of container,
Subsequent ultrasonic amplitude transformer immersed in liquid level is facilitated to carry out ultrasound, container is preferably polypropylene material centrifuge tube herein, chemistry and temperature
Performance is stablized, and being separated by filtration for subsequent ultrasonic treatment fluid is more favorable for.
Preferably, the quantity of the centrifuge tube 22 is 4-8, such as can be 4,5,6,7 or 8, preferably
It is 6.
Ultrasonic cell disruption instrument is mostly made of supersonic generator and energy converter two parts in the prior art, predominantly more
It plants the broken demand of animals and plants, virus, cell, bacterium and tissue and designs production, therefore most markets type on sale is
Single channel, flux is small, and integration is poor, and volume is big, and two parts conjunction weighs about 20~25kg, is not able to satisfy heavy metal member in cereal
The current Grain Trade demand of element and form field screening equipment high throughput portability.The present invention is by redesigning electronic control unit
Circuit structure, integrate driving unit and ultrasound unit, by its integration, keep the device integrated level higher, the smaller convenience of volume
It carries.Extraction flux is improved by the way of more ultrasonic amplitude transformers simultaneously, can extract 6 samples simultaneously, extraction efficiency is significant
It improves.
Preferably, the length of the ultrasonic amplitude transformer 211 is 8~10mm, such as can be 8mm, 9mm or 10mm.
Preferably, the depth that the ultrasonic amplitude transformer 211 immerses in sample liquid is 5mm.
The third aspect, the present invention provide a kind of extraction element as described in second aspect in extracting sample in mercury shape
Using.
Preferably, the matrix of the sample is cereal, including barley, wheat, highland barley, rye, oat, soybean, red bean, green
Any one of beans, rice, corn, sorghum or buckwheat or at least two mixing, preferably rice.
Compared with prior art, the invention has the following beneficial effects:
(1) method of mercury shape is fast and convenient in present invention extraction cereal, and sample is not necessarily to soaked overnight, tries without using soda acid
Agent, without before upper machine testing heating catch up with acid or adjust extracting liquid pH value, extractant is L-cysteine, to human body and environment without
Harm is three kinds of inorganic mercury, methyl mercury and ethyl mercury mercury shapes in extractable sample using ultrasonication 5min, and recovery rate can
Up to 95% or more；
(2) present invention is based on ultrasonication principle, according to mercury shape rapid extracting method main points in the cereal of foundation,
A kind of high-throughput Portable heavy metal extract equipment is developed, six channels can be reached while being extracted, by redesigning integrated electricity
Path control system, each assembly material and assembling form, add level sensor, are equipped with great Rong under the premise of keeping mains supply
Battery is measured, keeps device integration, automation and portable degree higher, fills up Grain Trade total metals and form scene sieve
The rapidly extracting equipment notch looked into；
(3) by mercury shape rapid extracting method in the cereal of the invention established and the high-throughput Portable heavy metal developed
The mating popularization of extract equipment, it is practical to solve the problems, such as total metals and form scene rapidly extracting in industry, to Grain Trade
The fast development of heavy metal field screening is of great significance.
Detailed description of the invention
Fig. 1 is the extraction element structural schematic diagram of mercury shape in rapidly extracting cereal in embodiment 1, wherein 1 is that driving is single
Member, 11 be drive shaft, and 12 be motor, and 2 be ultrasound unit, and 21 be ultrasonic head, and 211 be ultrasonic amplitude transformer, and 22 be centrifuge tube, and 3 are
Electronic control unit, 4 be display unit, and 5 be belt, and 6 be liquid level sensor, and 7 be pan straddle, and 8 be battery.
Specific embodiment
Further to illustrate technological means and its effect adopted by the present invention, below by way of specific embodiment come into
One step illustrates technical solution of the present invention, but the present invention is not limited in scope of embodiments.
The extraction element of mercury shape in 1 rapidly extracting cereal of embodiment
As shown in Figure 1, the extraction element of rapidly extracting cereal mercury shape of the present invention include driving unit 1, ultrasound unit 2,
Electronic control unit 3 and display unit 4, the driving unit 1 are connected by belt 5 with ultrasound unit 2, the driving unit 1, ultrasound
Unit 2, display unit 4 are connect with electronic control unit 3 respectively；
The driving unit 1 includes drive shaft 11 and motor 12, and the drive shaft 11 is connected directly with motor 12, motor 12
It is energized by battery 8；
The ultrasound unit 2 includes ultrasonic head 21 and sample container centrifuge tube 22, and the ultrasound head 21 includes that 6 ultrasounds become
Width bar 211, corresponding with 6 sample containers 22 respectively to place, sample container 22 is placed on pan straddle 7.A length of 32cm of device,
Wide 25cm, high 30cm.
The working principle of extraction element of the present invention is as follows:
It is crushed to 0.25mm after brown rice is shelled, 0.5g is taken to be placed in sample container 22, half Guang of L- of 5mL 0.1% is added
Propylhomoserin solution, drive shaft 11 improve 7 position of pan straddle by belt 5, detect ultrasonic amplitude transformer 211 by liquid level sensor 6
Ultrasonic power 120W, ultrasonic 10s interval 2s, total 5min, by sample container 22 is arranged by display unit 4 in 5mm under immersed in liquid level
Middle extracting solution crosses 0.22 μm of aperture filter membrane after 4000rmp is centrifuged 5min, takes supernatant to be measured.
Mercury shape in 2 test sample of embodiment
Using the inorganic mercury and methyl in liquid chromatogram-atomic fluorescence spectrophotometry combined instrument detection 1 gained prepare liquid of embodiment
Mercury, and control group is set, it is specific as follows:
Control group weighs brown rice sample 0.5g in the same manner as in Example 1, according to GB5009.17-2014 " food safety state
The measurement of total mercury and organic mercury in family's standard food " as defined in pre-treating method extract, it is 5mol/L that 5mL concentration, which is added,
Hydrochloric acid is stood overnight；Ultrasonic water bath extracts 60min at room temperature, and during which shaking is for several times；4 DEG C are centrifuged 15min with 8000rmp；It draws
2mL supernatant is added dropwise the sodium hydroxide solution that mass fraction is 24% and adjusts pH to 5, and the L- half of 0.1mL10 g/L is added
Cystine solution, is finally settled to 5mL with ultrapure water；It is to be measured after 0.45 μm of organic membrane filtration.
1 gained prepare liquid of embodiment and control group are subjected to same detection, testing conditions are as shown in table 1, and testing result is such as
Shown in table 2.
Table 1
Table 2
As shown in Table 2, it will test result to be compared with the result that the existing national standard method of GB50019.17-2014 measures,
Show that there was no significant difference (P < 0.1) for the two testing result.
In conclusion the method that the present invention extracts mercury shape in cereal is fast and convenient, sample is not necessarily to soaked overnight, extractant
For L-cysteine, acid or adjusting extracting liquid pH value are caught up with without heating before upper machine testing, it is non-hazardous to human body and environment, it utilizes
Ultrasonication 5min is three kinds of inorganic mercury, methyl mercury and ethyl mercury mercury shapes in extractable sample, recovery rate up to 95% with
On；The present invention develops a kind of high-throughput Portable heavy metal extract equipment based on ultrasonication principle, integrated level, automatic
Change and portable degree is high, it is practical to solve the problems, such as total metals and form scene rapidly extracting in industry, to Grain Trade
The fast development of heavy metal field screening is of great significance.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. the extracting method of mercury shape in a kind of cereal, which is characterized in that described method includes following steps:
Grain sample and L-cysteine solution are mixed, mercury shape is extracted after ultrasonication, insoluble substance is removed, takes supernatant
Liquid is to be measured.
2. the method according to claim 1, wherein the method also includes pre-treatment steps: by grain sample
It crushes；
Preferably, the smashed partial size of the grain sample is less than 0.5mm, preferably 0.2~0.3mm.
3. method according to claim 1 or 2, which is characterized in that the mass fraction of the L-cysteine be 0.05~
0.5%；
Preferably, the volume mass ratio of the L-cysteine solution and grain sample is greater than 10:1.
4. method according to claim 1-3, which is characterized in that the instrument of the ultrasound is broken for supersonic cell
Broken instrument；
Preferably, the power of the ultrasound is 100~150W；
Preferably, the mode of the ultrasound is interval ultrasound, and ultrasonic 10s stops 1~5s；
Preferably, the time of the ultrasound is 3~5min.
5. method according to claim 1-4, which is characterized in that the mercury shape includes total mercury, inorganic mercury, first
Base mercury and ethyl mercury.
6. method according to claim 1-5, which is characterized in that it is described removal insoluble substance method include
It stands, be centrifuged or filter；
Preferably, the revolving speed of the centrifugation is 4000~20000rpm；
Preferably, the time of the centrifugation is 2~15min；
Preferably, the filter membrane being filtered into using aperture less than 0.45 μm is filtered, and preferably 0.2~0.3 μm.
7. method according to claim 1-6, which is characterized in that the method also includes detection total mercury and mercury shapes
The step of state；
Preferably, the method for the detection total mercury includes atomic absorption spectrography (AAS), atomic fluorescence spectrometry, inductively coupled plasma
Constitution spectrometry, inductively coupled plasma emission spectrography, spectrophotometer method or electrochemical process；
The method of the detection mercury shape includes liquid chromatogram-inductivity coupled plasma mass spectrometry method for combined use or liquid chromatogram-
Atomic fluorescence spectrophotometry method for combined use.
8. the extraction element of mercury shape in a kind of cereal, which is characterized in that the extraction element is used as claim 1-7 is any
Method described in extracts mercury shape from cereal；
The extraction element includes driving unit (1), ultrasound unit (2), electronic control unit (3) and display unit (4)；
The driving unit (1) is connected by transmission device with ultrasound unit (2), the driving unit (1), ultrasound unit (2),
Display unit (4) is connect with electronic control unit (3) respectively；
The driving unit includes drive shaft (11) and motor (12), and the drive shaft (11) is connected directly with motor (12)；
The ultrasound unit includes ultrasonic head (21), pan straddle (7), and the ultrasound head (21) includes ultrasonic amplitude transformer (211).
9. extraction element according to claim 8, which is characterized in that a length of 30~50cm of the extraction element, width are
20~40cm, a height of 30~50cm；
Preferably, the transmission device is belt (5)；
Preferably, the pan straddle (7) is connected with liquid level sensor (6)；
Preferably, the sample container includes centrifuge tube (22)；
Preferably, the quantity of the centrifuge tube (22) is 4~8；
Preferably, the length of the ultrasonic amplitude transformer (211) is 8~10cm.
10. a kind of application of extraction element as claimed in claim 8 or 9 in extracting sample in mercury shape；
Preferably, the matrix of the sample be cereal, including barley, wheat, highland barley, rye, oat, soybean, red bean, mung bean,
Any one of rice, corn, sorghum or buckwheat or at least two mixing.
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| CN111307549A (en) * | 2020-03-18 | 2020-06-19 | 国家粮食和物资储备局科学研究院 | Method for rapidly extracting multiple elements from grains |
| CN113777084A (en) * | 2021-09-07 | 2021-12-10 | 山东省环境保护科学研究设计院有限公司 | Method for detecting alkyl mercury in solid waste |
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| CN111307549A (en) * | 2020-03-18 | 2020-06-19 | 国家粮食和物资储备局科学研究院 | Method for rapidly extracting multiple elements from grains |
| CN111307549B (en) * | 2020-03-18 | 2023-03-14 | 国家粮食和物资储备局科学研究院 | Method for rapidly extracting multiple elements from grains |
| CN113777084A (en) * | 2021-09-07 | 2021-12-10 | 山东省环境保护科学研究设计院有限公司 | Method for detecting alkyl mercury in solid waste |
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