CN109142591A - The hydro-thermal extracting method and Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide are remained in a kind of tobacco - Google Patents
The hydro-thermal extracting method and Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide are remained in a kind of tobacco Download PDFInfo
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- CN109142591A CN109142591A CN201811315079.1A CN201811315079A CN109142591A CN 109142591 A CN109142591 A CN 109142591A CN 201811315079 A CN201811315079 A CN 201811315079A CN 109142591 A CN109142591 A CN 109142591A
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- maleic hydrazide
- tobacco
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- tandem mass
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The present invention relates to hydro-thermal extracting methods and Liquid Chromatography-Tandem Mass Spectrometry measuring method that maleic hydrazide is remained in a kind of tobacco, belong to Detecting Pesticide technical field in tobacco.The hydro-thermal extracting method includes the following steps: offal sample and hydrochloric acid to be centrifuged after being cooled to room temperature in extracting 1 ~ 3h under the conditions of 100 ~ 150 DEG C, supernatant is then crossed column purification, be washed with water it is de- to obtain the final product；It is characterized by: device therefor is hydrothermal reaction kettle when extraction.The present invention has the advantages that extracting method carries out in hydrothermal reaction kettle, it is easy to operate, quick, extraction efficiency is high, safety is good, and substantially increase sample processing throughput, and, suitable for tobacco sample maleic hydrazide remaining abundant extraction and measurement good with the measurement result consistency of International Standards Method.And the present invention carries out matrix with mark using maleic hydrazide blank tobacco sample when measuring Maleic Hydrazide Residues, and measurement result can be made more accurate.
Description
Technical field
The present invention relates to hydro-thermal extracting method and Liquid Chromatography-Tandem Mass Spectrometry measurement sides that maleic hydrazide is remained in a kind of tobacco
Method belongs to Detecting Pesticide technical field in tobacco.
Background technique
Maleic hydrazide, also known as maleic hydrazide, maleic acid hydrazide, maleic hydrazide are a plant growth regulators, are answered extensively
For tobacco to inhibit axillary bud growth.Although having no exact research achievement now proves that the use of maleic hydrazide can induce cancer
Disease, but have confirmed that large dosage ground will lead to gene mutation using maleic hydrazide.In the guiding residue limits that CORESTA is formulated
(GRLs) and in tobacco parent company of China company standard " YQ 50-2014 tobacco leaf pesticide maximum residue limit ", to maleic hydrazide in cigarette
Maximum residue limit in grass is set to 80mg/kg.After maleic hydrazide is applied to tobacco, it can be absorbed through blade face cuticula and enter and plant
Strain, a portion exist as free state, and another part then exists with glucosides reference state and the form in conjunction with lignin.
The maleic hydrazide of reference state is difficult directly to be extracted, and therefore, efficiently extracting remaining maleic hydrazide in tobacco is to its Accurate Determining
Premise.
It is International Standards Method ISO 4876- that the remaining extracting method of maleic hydrazide is remained in the tobacco reported at present earliest
1980(ISO method) steam distillation, after this method boils sample in lye, be added zinc granule, by hydrogen in statu nascendi will
Maleic hydrazide is reduced into succinic acid hydrazides, and then hydrolyzes, and steam distillation releases hydrazine, and spectrophotometry measures itself and 4- bis-
The yellow compound that methylamino benzaldehyde is formed.The extraction efficiency of this method is higher, can extract free state and reference state simultaneously
Maleic hydrazide, but the pre-treating method is more old, and process is complicated, is related to that reagent type is more, dosage is big, and a large amount of uses of highly basic
To extraction glass apparatus seriously corroded used.In recent years, develop it is many directly extracted with acidified methanol, mixed organic solvents it is straight
Connect extraction, hydrochloric acid solution heating and refluxing extraction, hydrochloric acid solution microwave auxiliary extraction pre-treating method from principle to the world mark
Quasi- pre-treating method improves.In contrast, hydrochloric acid solution can effectively facilitate the hydrolysis of glucosides reference state maleic hydrazide, recycling
Rate is higher, therefore application is also the most extensive.But need to be heated to reflux dress in these pre-treating methods extracted based on hydrochloric acid solution
It sets or microwave extracting apparatus, and leaves a question open to the extraction efficiency of the maleic hydrazide in conjunction with lignin.
It on the other hand, include ultraviolet-visible spectrophotometry, gas about the remaining measuring method of maleic hydrazide is remained in tobacco
Phase chromatographic mass spectrometry method, liquid chromatography and liquid chromatography tandem mass spectrometry.As Liquid Chromatography-Tandem Mass Spectrometry is in pesticide residue
Detection field it is universal, using sensitivity is higher and the better Liquid Chromatography-Tandem Mass Spectrometry of anti-interference ability, realize to tobacco
And in tobacco product Maleic Hydrazide Residues accurate qualitative and quantitative detection.
Invention CN201710785509.5 discloses the extraction of magnetic force heating stirring and the liquid phase color of maleic hydrazide in a kind of tobacco
Tandem mass spectrum detection method is composed, this method measurement result is suitable with ISO method, and it is more complete to the extraction of maleic hydrazide, but the party
Method is needed using magnetic heating stirrer and oil bath pan, and progress need to be sealed in pyroceram container, higher in bottle
Steam pressure will lead to bottle explosion danger, and a set of magnetic heating stirrer once only handles a sample.Working efficiency is low.This
Outside, in context of detection, standard working solution used in CN201710785509.5 is the matched standard working solution of pure solvent,
Not using bare substrate with mark, but also measurement result has certain deviation.
Summary of the invention
The primary purpose of the present invention is that the hydro-thermal extracting method that maleic hydrazide is remained in a kind of tobacco is provided, it is existing to solve
The technical problem of the extraction process complexity of maleic hydrazide is remained in technology tobacco.
Second object of the present invention is to provide the Liquid Chromatography-Tandem Mass Spectrometry measurement that maleic hydrazide is remained in a kind of tobacco
Method.
To achieve the above object, the technical scheme is that remaining the hydro-thermal extracting method of maleic hydrazide in a kind of tobacco,
The following steps are included: offal sample and hydrochloric acid are centrifuged, so under the conditions of 100 ~ 150 DEG C in extracting 1 ~ 3h after being cooled to room temperature
Supernatant is crossed into column purification afterwards, is washed with water and takes off to obtain the final product；Wherein: device therefor is hydrothermal reaction kettle when extraction.
The column of crossing was C18Solid-phase extraction column.
Every 1g offal sample is corresponding to be added 10mL hydrochloric acid, and the concentration of the hydrochloric acid is 2 ~ 4mol/L, preferably 4mol/L.
Directly hydrothermal reaction kettle is placed in 100 ~ 150 DEG C of baking oven when extraction.
The centrifugation is with the revolving speed of 8000 rpm centrifugation 5min.
The Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide is remained in a kind of tobacco, comprising the following steps:
By offal sample and hydrochloric acid, deuterated maleic hydrazide inner mark solution under the conditions of 100 ~ 150 DEG C in hydrothermal reaction kettle extraction 1 ~
3h is centrifuged after being cooled to room temperature, supernatant is then crossed column purification, is washed with water de-, filters to obtain prepare liquid, prepare liquid is carried out
Ultra performance liquid chromatography-tandem mass spectrum measurement.
The concentration of the deuterated maleic hydrazide inner mark solution is 200 μ g/mL.
The water phase membrane filtration being filtered into using 0.45 μm.
The ultra performance liquid chromatography-tandem mass spectrum measurement condition are as follows: chromatographic column: Hypercarb Porous
Graphitic Carbon liquid-phase chromatographic column；Column temperature: 30 DEG C；Sample volume: 1 μ L；Mobile phase: mobile phase A: the water containing 1% HAc,
Mobile phase B: the acetonitrile containing 1% HAc carries out gradient elution；Flow velocity: 0.3 mL/min；Mass Spectrometry Conditions: ion source: electron spray electricity
From source, temperature: 150 DEG C；Capillary voltage: 3.0 kV；Remove solvent temperature degree: 300 DEG C；Go solvent stream fast: 650 L/h；Instead
Air blowing flow velocity: 50 L/h；Monitoring pattern: multiple-reaction monitoring；The gradient of the gradient elution are as follows: 0min, 100%A；8min,
85%A, 15%B；15min, 85%A, 15%B；16min, 10%A, 90%B；20min, 10%A, 90%B；21min, 100%A；36min,
100%A。
The above-mentioned water for containing 1% HAc refers to that the volume ratio of HAc and water is 1:99；The above-mentioned acetonitrile for containing 1% HAc refer to HAc with
The volume ratio of acetonitrile is 1:99.
In liquid chromatography tandom mass spectrometry determination, series standard working solution is prepared using bare substrate.
The hydro-thermal extracting method that maleic hydrazide is remained in tobacco of the invention dries offal sample and hydrochloric acid at 100 ~ 150 DEG C
In case, 1 ~ 3h is extracted in hydrothermal reaction kettle, is centrifuged after being cooled to room temperature, supernatant is then crossed into column purification, be washed with water de-
To obtain the final product, easy to operate, quick, extraction efficiency is high, and safety is good, and substantially increases sample processing throughput, is suitable for tobacco sample
The remaining batch quantity analysis of product maleic hydrazide.
The measuring method that maleic hydrazide is remained in tobacco of the invention, first extracts the maleic hydrazide in tobacco with hydrochloric acid,
Then ultra performance liquid chromatography-tandem mass spectrum measurement, inner mark method ration are carried out again.The survey of maleic hydrazide is remained in tobacco of the invention
Determine that method is simple, accurate, precision is high.
Great advantage of the present invention compared to CN201710785509.5 is: the present invention uses can 200 DEG C of heatproof, pressure resistance
Remaining maleic hydrazide in tobacco is extracted in the hydrothermal reaction kettle of 3MPa, extraction efficiency is high, and safety is good, and hydrothermal reaction kettle is set
It is extracted in baking oven, to also substantially increase sample processing throughput.In addition, in context of detection,
The standard working solution that CN201710785509.5 is used is the matched standard working solution of pure solvent, is not matched using bare substrate
Mark, the present invention carry out matrix with mark using maleic hydrazide blank tobacco sample.The results showed that when matching mark without using bare substrate
Measurement result ratio accompany target measurement result high by about 10% using bare substrate.Therefore very it is necessary to carry out bare substrate to match mark,
To guarantee the reliability to sample Maleic Hydrazide Residues measurement result, to avoid the mistake for whether meeting sample limitation requirement
Sentence.
Detailed description of the invention
Fig. 1 is the hydro-thermal extraction element schematic diagram that maleic hydrazide is remained in 1 tobacco of embodiment；
The matched standard working solution chromatogram of Fig. 2 bare substrate；
Fig. 3 is containing the remaining tobacco sample extracting solution chromatogram of maleic hydrazide.
Specific embodiment
Only invention is further described in detail for following embodiments, but does not constitute any limitation of the invention.
Instrument and reagent
Ultra performance liquid chromatography tandem mass spectrometer (Waters, US)；
Hydrothermal reaction kettle (Beijing is auspicious at great achievement experimental instruments and equipment limited)；
Milli-Q ultrapure water system (Millipore company of the U.S.)；
Maleic hydrazide and deuterated maleic hydrazide (German Dr. Ehrenstorfer company)；
Methanol, acetonitrile (chromatographically pure, J. T. Baker company of the U.S.),
37% hydrochloric acid (electron level, Duksan Pure Chemicals company of South Korea)；
Offal sample is international common experiment 17/1 sample of JETS of maleic hydrazide,
Embodiment 1
The hydro-thermal extracting method of maleic hydrazide is remained in the tobacco of the present embodiment, comprising the following steps:
Weighing 1.00g(and be accurate to 0.01g) offal sample is in the hydrothermal reaction kettle liner of 50mL, addition 100 μ L, 200 μ g/mL
Deuterated maleic hydrazide internal standard and 10mL 4mol/L aqueous hydrochloric acid solution, after closing the lid, liner is put into reaction kettle, tightens and is placed on
In baking oven, 150 DEG C are risen to by room temperature, 1h is extracted at a temperature of this, after being cooled to room temperature, extracting solution is poured into 50mL centrifuge tube
In, after being centrifuged 5min with the revolving speed of 8000 rpm, use C18Solid phase extraction column purifies supernatant, applied sample amount 2mL, uses
2mL water elution, gained scavenging solution through 0.45 μm of water phase membrane filtration to get.
The Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide is remained in the tobacco of the present embodiment, comprising the following steps:
1) preparation of prepare liquid
Weighing 1.00g(and be accurate to 0.01g) offal sample is in the hydrothermal reaction kettle liner of 50mL, addition 100 μ L, 200 μ g/mL
Deuterated maleic hydrazide internal standard and 10mL 4mol/L aqueous hydrochloric acid solution, after closing the lid, liner is put into reaction kettle, tightens and is placed on
In baking oven, 150 DEG C are risen to by room temperature, 1h is extracted at a temperature of this, after being cooled to room temperature, extracting solution is poured into 50mL centrifuge tube
In, after being centrifuged 5min with the revolving speed of 8000 rpm, use C18Solid phase extraction column purifies supernatant, applied sample amount 2mL, uses
2mL water elution, gained scavenging solution through 0.45 μm of water phase membrane filtration to get.
2) preparation of bare substrate
Weighing 1.00g(and be accurate to 0.01g) blank offal sample is in the hydrothermal reaction kettle liner of 50mL, addition 10mL 4mol/
After closing the lid, liner is put into reaction kettle, tightens and is placed in baking oven for L aqueous hydrochloric acid solution, 150 DEG C is risen to by room temperature, in this
At a temperature of extract 1h, after being cooled to room temperature, extracting solution is poured into 50mL centrifuge tube, 5min is centrifuged with the revolving speed of 8000 rpm
Afterwards, C is used18Solid phase extraction column purifies supernatant, applied sample amount 2mL, and with 2mL water elution, gained scavenging solution is through 0.45 μ
M water phase membrane filtration.Column was repeated, each blank sample can obtain about 12mL bare substrate, and 5 blank samples of parallel extraction will
Gained bare substrate mixes, and standard working solution to be prepared uses.
3) preparation of series standard working solution
The preparation of stock solution: the maleic hydrazide stock solution and 200 μ g/mL that mass concentration is about 100 μ g/mL are prepared using water as solvent
Deuterated maleic hydrazide inner mark solution.
The preparation of series standard working solution: accurately pipette respectively 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1.0mL and
The maleic hydrazide stock solution of the 100 μ g/mL of 2.0mL is separately added into the 200 μ g/mL's of 100 μ L in the volumetric flask of different 10mL
Deuterated maleic hydrazide inner mark solution dilutes constant volume with above-mentioned gained bare substrate, obtains series standard working solution, corresponding standard
The concentration of maleic hydrazide is 0.5 μ g/mL, 1 μ g/mL, 2 μ g/mL, 5 μ g/mL, 10 μ g/mL, 20 μ g/mL, sprout inhibition in working solution
Red content is 5 μ g, 10 μ g, 20 μ g, 50 μ g, 100 μ g, 200 μ g.
4) production of standard working curve
The series standard working solution of 6 kinds of concentration obtained by step 3) is subjected to ultra performance liquid chromatography-tandem mass spectrum measurement analysis,
With the ratio between the chromatographic peak area of object and interior target chromatographic peak area for ordinate, carried out by abscissa of the content of maleic hydrazide
Regression analysis obtains standard curve and its regression equation.The chromatogram of third level standard working solution is as shown in Figure 2.Standard work
It is as curveY=1.09241*X+ 0.262602(R 2 =0.999825).
The determination condition of above-mentioned ultra performance liquid chromatography-tandem mass spectrum are as follows: chromatographic condition: chromatographic column Hypercarb
Porous Graphitic Carbon liquid-phase chromatographic column (100mm × 4.6mm, 5 μm)；Column temperature: 30 DEG C；Sample volume: 1 μ L；Stream
Dynamic phase: mobile phase A: the water containing 1% HAc, Mobile phase B: the acetonitrile containing 1% HAc carries out gradient elution；Flow velocity: 0.3 mL/
min；Gradient is as shown in table 1.
1 gradient of table
| Time (min) | A(%) | B(%) |
| 0 | 100 | 0 |
| 8 | 85 | 15 |
| 15 | 85 | 15 |
| 16 | 10 | 90 |
| 20 | 10 | 90 |
| 21 | 100 | 0 |
| 36 | 100 | 0 |
Mass Spectrometry Conditions: ion source: electrospray ionisation source (ESI), temperature: 150 DEG C；Capillary voltage: 3.0 kV；Remove solvent temperature
Degree: 300 DEG C；Go solvent stream fast: 650 L/h；Blowback gas velocity: 50 L/h；Multiple-reaction monitoring pattern (MRM), detail parameters
It is shown in Table 2.
The UPLC-MS/MS MRM parameter of 2 maleic hydrazide of table and deuterated maleic hydrazide
* quota ion
5) ultra performance liquid chromatography of prepare liquid-tandem mass spectrum measurement
Prepare liquid obtained by step 1) is subjected to ultra performance liquid chromatography-tandem mass spectrum measurement, determination condition is the same as superelevation in step 4)
Effect liquid phase chromatogram-tandem mass spectrum determination condition.The color of the chromatographic peak area and internal standard compound of resulting target analytes will be measured
The ratio between spectral peak area substitutes into the resulting standard curve of step 4), and the content of maleic hydrazide in prepare liquid is calculated.Sample extraction
The chromatogram of liquid is as shown in Figure 3.
Experimental example 2
Respectively with International Standards Method (ISO method), CN201710785509.5 announce method (magnetic force heating stirring method) and
Maleic hydrazide in 6 offal samples of method of the invention common experiment JETS 17/1 international to maleic hydrazide is extracted and is surveyed
Fixed, the comparison of three kinds of method quantitative results is as shown in table 3.
The comparison (mg/kg) of 3 distinct methods measurement result of table
By 3 content of table it is found that the consistency of three kinds of method measurement results is preferable, and compared with classical International Standards Method, magnetic
The standard deviation of the measurement result of power heating stirring method and this method is relatively small.This method and magnetic force heating stirring method phase
Than with the high clear superiority of equipment safety, sample processing throughput.
Experimental example 3
Blank offal sample is carried out by 10,20, tri- pitch-based spheres of 50mg/kg and maximum residue limit (80 mg/kg)
Rate of recovery experiment, is measured in parallel 3 times, obtained relative recovery is in 95.6 ~ 102.9% ranges.In view of liquid chromatography tandem
Matrix effect when Mass Spectrometer Method adds to maleic hydrazide in blank offal through hydrothermal reaction kettle extraction and purified peak area
Divided by peak area equivalent maleic hydrazide being fed directly in bare substrate extracting solution, obtain absolute recovery in 72.8 ~ 75.9% models
In enclosing.It is gradually diluted with bare substrate by the matched minimum concentration standard working solution of bare substrate, is detection with 3 times of signal-to-noise ratio
Limit, 10 times of signal-to-noise ratio are quantitative limit, obtain the detection limit of this method are as follows: 0.68 mg/kg, quantitative limit are as follows: 2.27 mg/kg.This
Outside, it should be understood that accompanying target measurement result high using bare substrate with measurement result ratio when marking without using bare substrate
About 10%.Therefore very it is necessary to carry out bare substrate with mark, to guarantee to the reliable of sample Maleic Hydrazide Residues measurement result
Property, to avoid the erroneous judgement for whether meeting sample limitation requirement.
Claims (10)
1. remaining the hydro-thermal extracting method of maleic hydrazide in a kind of tobacco, comprising the following steps: by offal sample and hydrochloric acid 100 ~
It in extracting 1 ~ 3h under the conditions of 150 DEG C, is centrifuged after being cooled to room temperature, supernatant is then crossed into column purification, be washed with water and take off to obtain the final product；Its
Be characterized in that: device therefor is hydrothermal reaction kettle when extraction.
2. in tobacco according to claim 1 remain maleic hydrazide hydro-thermal extracting method, which is characterized in that it is described cross column be
Cross C18Solid-phase extraction column.
3. remaining the hydro-thermal extracting method of maleic hydrazide in tobacco according to claim 1, which is characterized in that every 1g offal sample
Product are corresponding to be added 10mL hydrochloric acid, and the concentration of the hydrochloric acid is 2 ~ 4mol/L.
4. remaining the hydro-thermal extracting method of maleic hydrazide in tobacco according to claim 1, which is characterized in that direct when extraction
Hydrothermal reaction kettle is placed in 100 ~ 150 DEG C of baking oven.
5. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide in a kind of tobacco, which comprises the following steps:
By offal sample and hydrochloric acid, deuterated maleic hydrazide inner mark solution under the conditions of 100 ~ 150 DEG C in hydrothermal reaction kettle extraction 1 ~
3h is centrifuged after being cooled to room temperature, supernatant is then crossed column purification, is washed with water de-, filters to obtain prepare liquid, prepare liquid is carried out
Ultra performance liquid chromatography-tandem mass spectrum measurement.
6. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide in tobacco according to claim 5, feature exists
In every 1g offal sample is corresponding to be added 10mL hydrochloric acid, and the concentration of the hydrochloric acid is 2 ~ 4mol/L；The deuterated maleic hydrazide internal standard is molten
The concentration of liquid is 200 μ g/mL.
7. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide in tobacco according to claim 5, feature exists
In the water phase membrane filtration being filtered into using 0.45 μm.
8. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide in tobacco according to claim 5, feature exists
In the ultra performance liquid chromatography-tandem mass spectrum measurement condition are as follows: chromatographic column: Hypercarb Porous Graphitic
Carbon liquid-phase chromatographic column；Column temperature: 30 DEG C；Sample volume: 1 μ L；Mobile phase: mobile phase A: Mobile phase B: the water containing 1% HAc contains
The acetonitrile of 1% HAc carries out gradient elution；Flow velocity: 0.3 mL/min；Mass Spectrometry Conditions: ion source: electrospray ionisation source, temperature:
150℃；Capillary voltage: 3.0 kV；Remove solvent temperature degree: 300 DEG C；Go solvent stream fast: 650 L/h；Blowback gas velocity: 50
L/h；Monitoring pattern: multiple-reaction monitoring；The gradient of the gradient elution are as follows: 0min, 100%A；8min, 85%A, 15%B；
15min, 85%A, 15%B；16min, 10%A, 90%B；20min, 10%A, 90%B；21min, 100%A；36min, 100%A.
9. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide, feature in the tobacco according to claim 5 or 8
It is, in liquid chromatography tandom mass spectrometry determination, series standard working solution is prepared using bare substrate.
10. remaining the Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide in tobacco according to claim 9, feature exists
In, the bare substrate the preparation method is as follows:
Weighing 1.00g(and be accurate to 0.01g) blank offal sample is in the hydrothermal reaction kettle liner of 50mL, addition 10mL 4mol/
After closing the lid, liner is put into reaction kettle, tightens and is placed in baking oven for L aqueous hydrochloric acid solution, 150 DEG C is risen to by room temperature, in this
At a temperature of extract 1h, after being cooled to room temperature, extracting solution is poured into 50mL centrifuge tube, 5min is centrifuged with the revolving speed of 8000 rpm
Afterwards, C is used18Solid phase extraction column purifies supernatant, applied sample amount 2mL, and with 2mL water elution, gained scavenging solution is through 0.45 μ
M water phase membrane filtration；Column was repeated, each blank sample can obtain about 12mL bare substrate, and 5 blank samples of parallel extraction will
Gained bare substrate mixes, and standard working solution to be prepared uses.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110954679A (en) * | 2019-12-24 | 2020-04-03 | 陕西华邦检测服务有限公司 | Extraction method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101876649A (en) * | 2010-07-02 | 2010-11-03 | 中国烟草总公司郑州烟草研究院 | Method for measuring residual maleic hydrazide in tobacco or tobacco product |
| CN102092725A (en) * | 2010-12-01 | 2011-06-15 | 西南科技大学 | Method for producing hydrate crystal silicon sodium titanate from waste strontium-barium glass |
| CN103472146A (en) * | 2013-08-19 | 2013-12-25 | 广东电网公司电力科学研究院 | Method for measuring content of chloridion and fluorinion in solid biomass fuel |
| CN106065036A (en) * | 2016-07-19 | 2016-11-02 | 西北农林科技大学 | A kind of hydro-thermal method extracts the method for tea polysaccharide |
| CN107589187A (en) * | 2017-09-04 | 2018-01-16 | 国家烟草质量监督检验中心 | One grow tobacco it is middle residual maleic hydrazide extracting method and assay method |
-
2018
- 2018-11-06 CN CN201811315079.1A patent/CN109142591A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101876649A (en) * | 2010-07-02 | 2010-11-03 | 中国烟草总公司郑州烟草研究院 | Method for measuring residual maleic hydrazide in tobacco or tobacco product |
| CN102092725A (en) * | 2010-12-01 | 2011-06-15 | 西南科技大学 | Method for producing hydrate crystal silicon sodium titanate from waste strontium-barium glass |
| CN103472146A (en) * | 2013-08-19 | 2013-12-25 | 广东电网公司电力科学研究院 | Method for measuring content of chloridion and fluorinion in solid biomass fuel |
| CN106065036A (en) * | 2016-07-19 | 2016-11-02 | 西北农林科技大学 | A kind of hydro-thermal method extracts the method for tea polysaccharide |
| CN107589187A (en) * | 2017-09-04 | 2018-01-16 | 国家烟草质量监督检验中心 | One grow tobacco it is middle residual maleic hydrazide extracting method and assay method |
Non-Patent Citations (2)
| Title |
|---|
| 李杰 等: "水热法提取金银花中绿原酸的工艺研究", 《食品研究与开发》 * |
| 边照阳 等: "《烟草农药残留分析技术》", 31 January 2015, 中国轻工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110954679A (en) * | 2019-12-24 | 2020-04-03 | 陕西华邦检测服务有限公司 | Extraction method |
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Application publication date: 20190104 |