CN108508104A - A kind of method of aldehydes matter in measurement main flume - Google Patents
A kind of method of aldehydes matter in measurement main flume Download PDFInfo
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- CN108508104A CN108508104A CN201810147259.7A CN201810147259A CN108508104A CN 108508104 A CN108508104 A CN 108508104A CN 201810147259 A CN201810147259 A CN 201810147259A CN 108508104 A CN108508104 A CN 108508104A
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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
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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
- G01N30/14—Preparation by elimination of some components
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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
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- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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- 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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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
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- 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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of methods of aldehydes matter in measurement main flume, use following device:Sample extraction bottle, including:Outer tube (1), inner sleeve (2), catheter (4), sieve plate;Sample extraction frame (5);Sample collection frame (6);Turn to take out (7) and lower platen (8).Step is:1. collecting total particulate matter in mainstream smoke;2. filtering;3. collecting sample filtrate;4. being measured using liquid chromatography.The assay method of the present invention can be used for detecting the content of aldehydes matter in main flume, have the advantages that pre-treatment is simple and convenient, reproducible.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a method of measuring aldehydes matter in main flume.
Background technology
Simple phenolic compound (phenol, benzenediol, methylphenol etc.) is that one kind in cigarette mainstream flue gas is important harmful
Ingredient, they not only have compared with niff, it is difficult to be blanked, harmful effect is generated to cigarette sensory evolution;But also to skin
Skin and respiratory mucosa have strong impulse effect and carcinogenesis.Such compound, which is put into Canadian government and is included in 46 kinds, to be had
Evil ingredient list, and the control ingredients list of suggestion is classified as by the World Health Organization " tobacco product control research group ".Therefore
Aldehydes matter improves the suction quality of cigarette very for reducing the harmful components in cigarette in Accurate Determining cigarette mainstream flue gas
It is important.
The measurement of aldehydes matter mainly has liquid chromatography, gas chromatography, connected neighbor set, spectrophotometry
Deng.Peak when can only measure the total amount of phenols with connected neighbor set and spectrophotometry, and directly be measured using gas-chromatography
Type easily trails, and generally requires and uses derivatization.Liquid chromatography is since separative efficiency is high, selectivity is good, detection sensitivity is high, operation
Automation is widely applied in the analysis of simple phenolic compound.China tobacco business standard YC/T255-2008 is used
Phenol in Compounds of Mainstream Smoke By Hplc, the method chromatographic isolation time is long, each sample need 40min with
On, the requirement that sample quickly measures cannot be met.
In carrying out main flume in the measurement of phenols, needs to find a kind of easier, quick analysis method, can criticize
Amount, high-throughput operation, realize and quickly, efficiently, accurately measure.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of side measuring aldehydes matter in main flume
Method is analyzed providing method for cigarette mainstream flue gas and is supported.The present invention also aims to provide a kind of extraction of collection, filtering and transfer
The pretreating device being integrated can effectively realize that the batch processing of aldehydes matter and analysis measure in main flume.
The purpose of the present invention is what is be achieved by the following technical programs.
A kind of method of aldehydes matter in measurement main flume, which is characterized in that use following device:
Sample extraction bottle, including:Outer tube 1, sealed bottom and to be flat, oral area has a sealing ring 11;Inner sleeve
2, outer diameter is adapted with the internal diameter of the outer tube 1, length be more than the outer tube 1 length;Catheter 4, is located at
In the inner sleeve 2, lower end has an extension mouth and the lower end inner wall of the inner sleeve 2 to be sealedly and fixedly connected, and described interior
2 upper port of casing is fixedly connected to form compression face 21, and upper part is stretched out outside the inner sleeve 2, and back bending is downward;Sieve plate 3, position
In in the lower ending opening of the inner sleeve 2, for one or more;Sample extraction frame 5 inside has several sample extraction bottle putting holes
51, for placing the sample extraction bottle;Sample collection frame 6 inside has several sample bottle putting holes 61 and several waste collections
Bottle putting hole 62, for placing sample bottle 610 and waste collection bottle 620;Turn to take out 7, is located at 6 central part of sample collection frame;
The sample collection frame 6 and the sample extraction frame 5 can surround the pumping 7 that turns and rotate respectively;Lower platen 8, surface is extended with
Several push-down heads 81;
This approach includes the following steps:
1. according to condition smoking cigarette as defined in standard GB/T 19609-2004 and collecting total particulate matter in mainstream smoke, each
Cambridge filter collects 4 cigarette smokes;It takes the cambridge filter for gathering main flume to be placed in the outer tube, extraction examination is added
Agent is inserted into inner sleeve and is placed on the sample extraction frame 5 and carries out ultrasonic extraction;
2. being fixed using shaft, the nozzle of the catheter is made to be directed at waste collection bottle 620, push inner sleeve by
Pressure surface 21 simultaneously enters in catheter after so that extraction solution is passed through filtering sieve plate filtering, and passes out into waste collection bottle 620
In, initial filtrate 2-3mL enters in waste collection bottle 620;
3. centered on shaft, sample extraction frame is rotated, the downward back bending nozzle of the catheter is made to be directed at the sample
610 bottlenecks of bottle continue the compression face 21 for pushing inner sleeve, 1~1.5mL sample filtrates are transferred in sample bottle 610, are cooled to
Room temperature obtains sample filtrate to be analyzed;
4. being measured using liquid chromatography, quantified using peak area method, aldehydes matter in contrast sample filtrate
Peak area and standard solution working curve peak area method, you can determine the content of the aldehydes matter in main flume sample.
The aldehydes matter measured is:P- benzenediol, m- benzenediol, catechol, phenol, p-Cresol, m-cresol,
O-cresol.
Preferably, the step acetic acid aqueous solution that 1. extraction agent is 1v/v%.
Preferably, the aperture of the step 2. sieve plate is 0.45 μm.
Preferably, 4. the liquid phase chromatogram condition is step:Liquid phase chromatogram condition:ACQUITYUPLC BEH C18 colors
Compose column (50mm × 2.1mm, 1.7 μm);Column temperature:30℃;Column flow rate:0.5mL/min;Sample size:5.0μL;Mobile phase A:1v/
The acetic acid aqueous solution (including 0.01mol/L β-CD) of v%;Mobile phase B:70v/v% acetonitrile (include 1v/v% acetic acid and
0.01mol/Lβ-CD);Gradient elution;Using fluorescence detector program wavelength detecting.
Preferably, the liquid phase condition of gradient elution is:0~1.5min, 10v/v% Mobile phase B;1.5~3.0min,
10~40v/v% Mobile phase Bs;3.0~4.5min, 40~80v/v% Mobile phase B;4.5~5.0min, 80v/v% Mobile phase B;
5.0~5.5min, 10v/v% Mobile phase B;5.5~7.5min, 10v/v% Mobile phase B;Fluorescence program wavelength detecting:Detect wave
It is a length of:0~1.5min, excitation wavelength/launch wavelength are 284/332nm;1.5~2.0min, excitation wavelength/launch wavelength are
275/315nm;2.0~2.8min, excitation wavelength/launch wavelength are 277/319nm;2.8~3.8min, excitation wavelength/transmitting
Wavelength is 272/309nm;3.8-6.0min, excitation wavelength/launch wavelength are 273/323nm.
The method of the present invention integrates extraction, filtering, transfer using sample extraction bottle, and sample extracts in outer tube 1
After;Inner sleeve 2 is firmly pushed at compression face 21, extract liquor enters after being filtered by sieve plate 3 in catheter 4, and from
The downward mouth of back bending of catheter 4 exits into sample bottle, obtains sample filtrate and carries out chromatography.The extraction of this process sample
It takes, filter, shifting and be integrated, avoiding experimental error caused by operation.
1 oral area of outer tube dress fixes inner sleeve 2 there are one sealing ring 11 when for extracting, with prevent extract liquor from splashing out with
And it is buffered when sample filtering.
In the present invention, 4 diameter of catheter is preferably 1-2mm.
It is as follows using multiple sample extraction bottle operating process of apparatus of the present invention:Several sample extraction bottles (such as five) are put
In the extraction flask putting hole 51 for entering sample extraction frame 5, it is respectively put into sample and carries out extracting operation;Start the part solution collected
(such as 2ml) is abandoned, therefore is started first respectively the waste collection bottle 620 on the downward back bending of catheter 4 alignment sample collection frame 6
Oral area, lower platen 8 is covered, push-down head 81 is made to be respectively aligned to compression face 21, the liquid in waste collection bottle 620 reaches requirement
Afterwards, rotation sample extraction frame 5 or sample collection frame 6 make the downward back bending of catheter 4 be directed at the oral area of sample bottle 610, continue to
Lower platen 8 is pushed, the fluid sample in five sample extraction bottles enters respective drain after being filtered respectively by respective sieve plate 3
It in pipe 4, enters back into sample bottle 610, continues to push the bottom that the lower platen 8 makes inner sleeve 2 be depressed into outer tube 1, then institute
There is the liquid in sample extraction bottle to be transferred to respectively in sample bottle 610 by respective catheter 4, completes sample transfer behaviour
Make.Sample in sample bottle 610 can be respectively used to analyze.
Beneficial effects of the present invention are:
(1) device that uses of the present invention, need not shift in the pretreatment process of sample sample can directly extract, mistake
It filters and collects to obtain sample to be analysed, effectively prevent operating caused experimental error.Phenolic material in main flume of the present invention
The assay method of matter improves 5 times or more of determination efficiency, is suitable for the accurate test of batch samples;With it is simple, conveniently,
The advantages that effect of extracting is good, sample processing throughput is high.
(2) assay method sample extraction effect and precision of the invention improve a lot than conventional method, analysis knot
Fruit is consistent with the result that standard method measures.Have the advantages that quantitatively accurate, reproducible, detection limit is low etc., is suitable for large quantities of
Measure the accurate test of sample.The assay method sample analysis efficiency improves a lot than conventional method, can be phenol in main flume
The detection of substance provides accurately and reliably method, and effective technical support is provided for cigarette product evaluation.
Description of the drawings
Fig. 1 is the outer tube schematic diagram of the present invention;
Fig. 2 is the inner sleeve schematic diagram of the present invention;
Inner sleeve is inserted into housing spout part schematic diagram when Fig. 3 is the extraction mixing of the present invention;
Inner sleeve is inserted into outer tube schematic internal view when Fig. 4 is the extract liquor filtering of the present invention, transfer;
Fig. 5 is the sample extraction frame and sample collection frame schematic diagram of the present invention;
Fig. 6 is that the sample extraction bottle of the present invention is placed on sample extraction frame and sample collection bottle is placed on sample receipts
Collect the schematic diagram of sample transfer step when on frame;
Fig. 7 is the transparent lower platen schematic diagram of the present invention;
Fig. 8 is aldehydes matter standard solution chromatogram;
The chromatogram of aldehydes matter in 1 sample solution of Fig. 9 embodiments.
Description of the drawings:1- outer tubes;2- inner sleeves;21- compression faces;3- sieve plates;4- catheters;5- sample extraction framves;51-
Sample extraction bottle putting hole;6- sample collection framves;61- sample bottle putting holes;62- waste collection bottle putting holes;610- samples are received
Collect bottle;620- waste collection bottles;7- shafts;8- lower platens;81- push-down heads;82- handles;11- sealing rings;12- samples.
Specific implementation mode
Technical scheme of the present invention is described in detail with reference to embodiment, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of not making the creative labor, shall fall within the protection scope of the present invention.
In the examples where no specific technique or condition is specified, according to technology or condition described in document in the art or
Person carries out according to product description.Reagents or instruments used without specified manufacturer, being can be by buying the normal of acquisition
Advise product.
Embodiment 1
The method for measuring aldehydes matter in commercial cigarettes A main flumes, includes the following steps:
1. sample pre-treatments:Market commercial cigarettes A is randomly selected, is balanced under the conditions of as defined in GB/T 16447,
According to condition smoking cigarette as defined in standard GB/T 19609-2004 and total particulate matter in mainstream smoke is collected, each cambridge filter is received
Collect four cigarette smokes;It takes the cambridge filter for gathering main flume to be placed in outer tube, the acetic acid water of 50mL1v/v% is added
Inner sleeve is then stuck in the oral area of outer tube using sealing ring by solution;By eight samples of above-mentioned steps parallel processing.Then
Eight sample extraction pipes are placed on sample extraction frame and carry out ultrasonic extraction 35min;It is to be extracted completely after, carried out using shaft
It is fixed, make the downward mouth alignment waste collection bottle 620 of the back bending of respective catheter, then uses lower platen 8, push-down head 81 is made to divide
Not Dui Zhun compression face 21, apply downward power and push lower platen 8, make eight sample extraction solution respectively by respective sieves
Plate enters in catheter 4, and from 4 inner outflow of catheter, and initial filtrate 2mL enters waste collection bottle 620;Then in being with shaft
The heart, rotation sample extraction frame 5, makes, and makes the downward mouth alignment sample collection bottle 610 of the back bending of respective catheter, is pressed through under continuing
Inner sleeve is filtered, the solution 1mL of filtering is transferred in sample bottle;For liquid-phase chromatographic analysis.
2. liquid phase chromatogram condition is:Liquid phase chromatogram condition:ACQUITY UPLC BEH C18 chromatographic columns (50mm × 2.1mm,
1.7μm);Column temperature:30℃;Column flow rate:0.5mL/min;Sample size:5.0μL;Mobile phase A:The acetic acid aqueous solution of 1v/v% is (interior
- the CD of β containing 0.01mol/L);Mobile phase B:The acetonitrile (acetic acid and 0.01mol/L β-CD that include 1v/v%) of 70v/v%;Gradient
Elution, 0~1.5min, 10v/v% Mobile phase Bs;1.5~3.0min, 10~40v/v% Mobile phase B;3.0~4.5min, 40~
80v/v% Mobile phase Bs;4.5~5.0min, 80v/v% Mobile phase B;5.0~5.5min, 10v/v% Mobile phase B;5.5~
7.5min, 10v/v% Mobile phase B;Fluorescence program wavelength detecting:Detection wavelength is:0~1.5min, excitation wavelength/launch wavelength
For 284/332nm;1.5~2.0min, excitation wavelength/launch wavelength are 275/315nm;2.0~2.8min, excitation wavelength/hair
The a length of 277/319nm of ejected wave;2.8~3.8min, excitation wavelength/launch wavelength are 272/309nm;3.8-6.0min, excitation wave
Length/launch wavelength is 273/323nm.Using fluorescence detector program wavelength eight samples of Parallel testing, it is averaged.
It is obtained by detection, hydroquinone content is 68.57ug/ branch, resorcinol content in commercial cigarettes A main flumes
For 2.36ug/ branch, catechol content is 59.28ug/ branch, and phenol content is 18.22ug/ branch, and paracresol content is 8.36ug/
Branch, metacresol content are 7.27ug/ branch, and o-cresol content is 11.60ug/ branch.
Embodiment 2
Aldehydes matter in 4 kinds of commercial cigarettes B main flumes is measured, is included the following steps:
1. sample pre-treatments:It is balanced under the conditions of as defined in GB/T 16447, according to standard GB/T 19609-2004
Defined condition smoking cigarette simultaneously collects total particulate matter in mainstream smoke, and each cambridge filter collects four cigarette smokes;It takes and gathers
The cambridge filter of main flume is placed in outer tube, and the acetic acid aqueous solution of 50mL1v/v% is added, then, will be interior using sealing ring
Oral area of the casing clamp in outer tube;It is total to eight samples of parallel processing by above-mentioned steps.Then eight sample extraction pipes are placed on
Ultrasonic extraction 35min is carried out on sample extraction frame;It is to be extracted completely after, be fixed using shaft, make respective catheter
Back bending downward mouth alignment waste collection bottle 620, then uses lower platen 8, push-down head 81 is made to be respectively aligned to compression face 21, apply to
Under power push lower platen 8, so that eight sample extraction solution is entered in catheter 4 by respective filtering sieve plate respectively, and from
4 inner outflow of catheter, initial filtrate 2-3mL enter waste collection bottle 620;Then centered on shaft, sample extraction frame is rotated
5, make, makes the downward mouth alignment sample collection bottle 610 of the back bending of respective catheter, continue lower press filtration inner sleeve, by filtering
Solution is transferred in sample bottle;For liquid-phase chromatographic analysis.
2. liquid phase chromatogram condition is:Liquid phase chromatogram condition:ACQUITY UPLC BEH C18 chromatographic columns (50mm × 2.1mm,
1.7μm);Column temperature:30℃;Column flow rate:0.5mL/min;Sample size:5.0μL;Mobile phase A:The acetic acid aqueous solution of 1v/v% is (interior
- the CD of β containing 0.01mol/L);Mobile phase B:The acetonitrile (acetic acid and 0.01mol/L β-CD that include 1v/v%) of 70v/v%;Gradient
Elution, 0~1.5min, 10v/v% Mobile phase Bs;1.5~3.0min, 10~40v/v% Mobile phase B;3.0~4.5min, 40~
80v/v% Mobile phase Bs;4.5~5.0min, 80v/v% Mobile phase B;5.0~5.5min, 10v/v% Mobile phase B;5.5~
7.5min, 10v/v% Mobile phase B;Fluorescence program wavelength detecting:Detection wavelength is:0~1.5min, excitation wavelength/launch wavelength
For 284/332nm;1.5~2.0min, excitation wavelength/launch wavelength are 275/315nm;2.0~2.8min, excitation wavelength/hair
The a length of 277/319nm of ejected wave;2.8~3.8min, excitation wavelength/launch wavelength are 272/309nm;3.8-6.0min, excitation wave
Length/launch wavelength is 273/323nm.Using fluorescence detector program wavelength eight samples of Parallel testing, two of each sample
It is averaged, is averaged.
It is detected such as " this law " in table 1 using 4 kinds of cigarette of method pair of the present invention, and utilizes professional standard side simultaneously
Method is analyzed, as a result such as " rower ".The comparison of the two analysis result is shown in Table 1.
1 cigarette product phenols analysis result of table (μ g/ branch)
Testing result and professional standard measurement result of the invention are almost the same as can be seen from Table 1, but of the invention
As a result of high-throughput detection technique:Batch pretreatment technology and ultra-performance liquid chromatography, analysis testing efficiency is significantly
It improves, under the premise of ensureing analysis result accuracy, 5 times or more of determination efficiency can be improved than conventional method.
Claims (6)
1. a kind of method measuring aldehydes matter in main flume, which is characterized in that use following device:
Sample extraction bottle, including:Outer tube (1), sealed bottom and to be flat, oral area has a sealing ring (11);Inner sleeve
(2), outer diameter is adapted with the internal diameter of the outer tube (1), length be more than the outer tube (1) length;Catheter
(4), it is located in the inner sleeve (2), lower end has the lower end inner wall of an extension mouth and the inner sleeve (2) to seal fixed connect
It connecing, compression face (21) is fixedly connected to form with the inner sleeve (2) upper port, upper part stretches out inner sleeve (2) outside,
And back bending is downward;Sieve plate (3) is located in the lower ending opening of the inner sleeve (2), for one or more;Sample extraction frame (5),
There are several sample extraction bottle putting holes (51) in it, for placing the sample extraction bottle;Sample collection frame (6), if inside having
Dry-eye disease bottle putting hole (61) and several waste collection bottle putting holes (62), for placing sample bottle (610) and waste collection bottle
(620);Turn to take out (7), is located at sample collection frame (6) central part;The sample collection frame (6) and the sample extraction frame
(5) pumping (7) that turns can be surrounded respectively to rotate;Lower platen (8), surface are extended with several push-down heads (81);
This approach includes the following steps:
1. according to condition smoking cigarette as defined in standard GB/T 19609-2004 and collecting total particulate matter in mainstream smoke, each Cambridge
Filter disc collects 4 cigarette smokes;It takes the cambridge filter for gathering main flume to be placed in the outer tube, extraction agent is added,
It is inserted into inner sleeve and is placed on the sample extraction frame (5) and carry out ultrasonic extraction;
2. being fixed using shaft, so that the nozzle of the catheter is directed at waste collection bottle (620), push the compression of inner sleeve
Face (21) simultaneously enters in catheter after so that extraction solution is passed through filtering sieve plate filtering, and passes out into waste collection bottle
(620) in, initial filtrate 2-3mL enters in waste collection bottle (620);
3. centered on shaft, sample extraction frame is rotated, the downward back bending nozzle of the catheter is made to be directed at the sample bottle
(610) bottleneck continues the compression face (21) for pushing inner sleeve, 1~1.5mL sample filtrates is transferred in sample bottle (610), cold
But sample filtrate to be analyzed is obtained to room temperature;
4. being measured using liquid chromatography, quantified using peak area method, the peak of aldehydes matter in contrast sample filtrate
The peak area method of area and standard solution working curve, you can determine the content of the aldehydes matter in main flume sample.
2. according to the method described in claim 1, it is characterized in that, the step acetic acid water that 1. extraction agent is 1v/v%
Solution.
3. according to the method described in claim 1, it is characterized in that, the aperture of the step 2. sieve plate is 0.45 μm.
4. according to the method described in claim 1, it is characterized in that, step 4. the liquid phase chromatogram condition is:Liquid chromatogram
Condition:ACQUITYUPLC BEH C18 chromatographic columns (50mm × 2.1mm, 1.7 μm);Column temperature:30℃;Column flow rate:0.5mL/min;
Sample size:5.0μL;Mobile phase A:The acetic acid aqueous solution of 1v/v%;Mobile phase B:The acetonitrile of 70v/v%;Gradient elution;Using glimmering
Photodetector program wavelength detecting.
5. according to the method described in claim 4, it is characterized in that, the mobile phase A contains 0.01mol/L β-CD;The stream
Dynamic phase B contains the acetic acid and 0.01mol/L β-CD of 1v/v%.
6. according to the method described in claim 4, it is characterized in that, the liquid phase condition of gradient elution is:0~1.5min,
10v/v% Mobile phase Bs;1.5~3.0min, 10~40v/v% Mobile phase B;3.0~4.5min, 40~80v/v% Mobile phase B;
4.5~5.0min, 80v/v% Mobile phase B;5.0~5.5min, 10v/v% Mobile phase B;5.5~7.5min, 10v/v% flow
Phase B;Fluorescence program wavelength detecting:Detection wavelength is:0~1.5min, excitation wavelength/launch wavelength are 284/332nm;1.5~
2.0min, excitation wavelength/launch wavelength are 275/315nm;2.0~2.8min, excitation wavelength/launch wavelength are 277/319nm;
2.8~3.8min, excitation wavelength/launch wavelength are 272/309nm;3.8-6.0min, excitation wavelength/launch wavelength are 273/
323nm。
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Cited By (1)
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CN112504765A (en) * | 2020-10-20 | 2021-03-16 | 自然资源部第二海洋研究所 | Device and method for collecting submarine hydrothermal solution nozzle particles |
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CN101984352A (en) * | 2009-11-05 | 2011-03-09 | 中国烟草总公司郑州烟草研究院 | Method of measuring main phenolic compounds in primary smoke of cigarette |
CN102313782A (en) * | 2010-07-09 | 2012-01-11 | 福建中烟工业公司 | Method for rapid separation and determination of seven volatile phenols in flue gas of main cigarette flow |
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2018
- 2018-02-12 CN CN201810147259.7A patent/CN108508104A/en not_active Withdrawn
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