CN109459506A - A kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves - Google Patents
A kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves Download PDFInfo
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- CN109459506A CN109459506A CN201811160156.0A CN201811160156A CN109459506A CN 109459506 A CN109459506 A CN 109459506A CN 201811160156 A CN201811160156 A CN 201811160156A CN 109459506 A CN109459506 A CN 109459506A
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- hexane
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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
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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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
A kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves, it is characterized by: successively including the following steps: to weigh smashed Tea Samples in centrifuge tube, anhydrous sodium sulfate and n-hexane-acetone soln is added, be vortexed mixing, ultrasonic extraction, centrifugation, take supernatant, nitrogen blows concentration, then uses toluene constant volume, obtains Tea Samples solution to be clean；Functionalized multi-wall carbonnanotubes, PSA and anhydrous magnesium sulfate is added, is vortexed, centrifugation takes supernatant liquid nitrogen to blow close dry, is quantitatively adding n-hexane, is vortexed and mixes, and filter membrane obtains Tea Samples scavenging solution, analyzes for GC-MS.The present invention effectively reduces the interference of the impurity such as pigment in matrix, tea polyphenols, catechin, obtains preferable extraction efficiency and clean-up effect, and easy to operate, quick and precisely, high sensitivity.
Description
Technical field
The present invention relates to analytical chemistry fields, and in particular to a kind of quick sample pre-treatment detected for Polychlorinated biphenyls in tealeaves
Method, the quick sample pretreatment method are a kind of based on wanting dispersive solid-phase extraction adsorbent based on modified carbon nano tube tube material
Pre-treating method can be used for detecting 18 kinds of Polychlorinated biphenyls (PCBs) in tealeaves simultaneously in conjunction with gas chromatography-mass spectrum (GC-MS).
Background technique
Polychlorinated biphenyls (PCBs) is a kind of artificial synthesized askarel class aromatic compound, once as high-quality industry addition
The a large amount of uses of agent (heat carrier, fire retardant, plasticizer, insulating materials etc.) are in fields such as printing, chemical industry, electric power, plastics, paint.
Literature research shows that PCBs can result in organism endocrine disturbance, immune and reproductive system destroys, and induces cancer and nerve
Disease, 1970s start to stop production and use in the world, but in air, soil, water body, deposit, biology
It is constantly detected in the media such as sample, food, it has also become a kind of generally existing persistence organic pollutant is put into Si Dege
You control pollutant list at pact of rubbing in the first batch.
About the detection method of PCBs, mainly there are gas chromatography (GC-ECD), gas chromatography-mass spectrography (GC- at present
MS), gas chromatography tandem mass spectrometry method (GC-MS/MS) etc..The pretreatment technology of use has Soxhlet extraction, liquid-liquid extraction, acceleration
The abstraction techniques such as solvent extraction, microwave auxiliary extraction, supercritical fluid extraction and Solid Phase Extraction, gel permeation chromatography, H2SO4
The purification techniques such as sulfonation, solid phase microextraction, often process is cumbersome, time-consuming for these methods, and solvent-oil ratio is big, some extraction process
Special equipment is needed, analysis cost is higher.
Dispersive solid-phase extraction technology is easy to operate, quick, efficient, low in cost to have many advantages, such as, obtains in recent years
It rapidly develops, is widely applied in detection fields such as environment, food.The key and core of the technology are sorbent materials.Commonly
Adsorbent, such as N- propyl ethylenediamine (PSA), ketjenblack EC (GCB), C18, clean-up effect to complex matrices are simultaneously paid no attention to
Think, and price is relatively high.
Summary of the invention
The present invention provides a kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves, and its object is to solve
Clean-up effect present in certainly existing Tea Samples pre-treating method is undesirable, subsequent detection is vulnerable to impurity effect and preceding place
The problem of managing material therefor higher cost.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: it is a kind of in tealeaves Polychlorinated biphenyls detect it is fast
Fast sample-pretreating method, successively includes the following steps:
The first step weighs smashed Tea Samples in centrifuge tube, and anhydrous sodium sulfate and n-hexane-acetone soln is added, according to
It is secondary to carry out vortex mixing, ultrasonic extraction, centrifugation, then take supernatant into test tube, nitrogen blows concentration, is then settled to institute with toluene
Volume is needed, Tea Samples solution to be clean is obtained；Wherein, the mass ratio of the Tea Samples and anhydrous sodium sulfate is 1:1, tealeaves
The input ratio of sample and the n-hexane-acetone soln is that 10~20ml n-hexane-acetone is put into every 1g fresh tea leaves sample
Solution；
Modified carbon nano-tube, PSA and anhydrous magnesium sulfate are added into Tea Samples solution to be clean for second step, are vortexed, from
The heart takes supernatant liquid nitrogen to blow close dry, is quantitatively adding n-hexane, is vortexed and mixes, cross organic system filter membrane, obtain Tea Samples scavenging solution,
It is analyzed for GC-MS；Wherein, the modified carbon nano-tube is functionalized multi-wall carbonnanotubes, the Tea Samples, modified carbon nano tube
The mass ratio of pipe, PSA and anhydrous magnesium sulfate is 10:1~1.5:1~1.5:1.
Related content in above-mentioned technical proposal is explained as follows:
1, in above scheme, preferable scheme is that the volume ratio of n-hexane and acetone is 1:1 in the n-hexane-acetone soln.
2, in above scheme, preferable scheme is 10~20min of ultrasonic extraction in the first step, with 6000~
9000 r/min are centrifuged 2~8min.
3, in above scheme, preferable scheme be in the second step, with 7000~10000r/min centrifugation 2~
10min。
4, in above scheme, the functionalized multi-wall carbonnanotubes are called MWCNTs-COOH.
Design feature of the present invention: carbon nanotube is a kind of novel nano carbon material, very big due to having compared with PSA etc.
Specific surface area, adsorption capacity is higher, adsorptivity ability more preferably, relative low price, in recent years by as dispersive solid-phase extraction
Adsorbent is widely used in the samples such as water body, soil, food in the detection of each pollutant, effectively improves pre-treatment
Efficiency reduces the cost of detection.But carbon nanotube is used to more chlorine in tealeaves as dispersive solid-phase extraction adsorbent at present to join
There is not been reported for the detection of benzene (PCBs).
Sample-pretreating method of the invention is using tealeaves as object, and Tea Samples are mixed through acetone-n-hexane (1:1, v/v)
Bonding solvent extracts, and extracting solution solvent is replaced into toluene, then with the purification of MWCNTs-COOH and PSA mixed adsorbent, efficiently reduces
The interference of the impurity such as pigment, tea polyphenols, catechin, obtains preferable extraction efficiency and clean-up effect in matrix.Of the invention
Methodology Verification is good, each PCBs object linear correlation (r >=0.9998) within the scope of 0.005~0.5mg/kg,
For matrix recovery of standard addition between 90.7%~115.2%, RSD (n=5) is 0.005mg/kg no more than 10.9%, LOQ.
Sample-pretreating method of the invention uses adsorbent of the modified carbon nano-tube as dispersion solid-phase extraction method, can
It is established for combination GC-MS while detecting the analysis method of 18 kinds of PCBs in tealeaves.This method is easy to operate, good purification,
Accuracy is high, and stability is good, for guaranteeing that quality and safety of tea has positive meaning.
In short, the method for the present invention is easy to operate compared with conventional solid extracting process, and quick and precisely, high sensitivity, purification
Effect is good, easily formation normalizing operation, provides effective method to carry out the detection research of PCBs in tealeaves.
Detailed description of the invention
Attached drawing 1 is the GC-MS chromatogram that 18 kinds of PCBs mix standard liquid, and according to peak sequence, successively label, number designation divide
Not Biao Shi: 1.PCB28；2.PCB52；3.PCB101；4.PCB81；5.PCB77；6.PCB123；7.PCB118； 8.PCB114；
9.PCB153；10.PCB105；11.PCB138；12.PCB126；13.PCB167；14.PCB156； 15.PCB157；
16.PCB180；17.PCB169；18.PCB189.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments:
A kind of embodiment: quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves
The sample-pretreating method combination gas chromatography-mass spectrum (GC-MS) of the present embodiment detects chlorine more than 18 kinds in tealeaves simultaneously and joins
Benzene (PCBs), the specific detection method is as follows:
1, the preparation of standard solution:
Accurate 18 kinds of PCBs mixed standard solutions for measuring 1mL 10mg/L, with n-hexane constant volume, are made into 10mL volumetric flask
The hybrid standard mother liquor of 1mg/L is saved in 4 DEG C of refrigerator cold-storages；It puts before use, taking out to room temperature, is diluted step by step with n-hexane
At the hybrid standard working solution of 0.005,0.01,0.05,0.1 and 0.5mg/L.
Blank Tea Samples are taken, after pre-treatment, the mixing of 1.0mL various concentration is added with being dried with nitrogen in upper press proof liquid
Standard working solution, oscillation mix, and cross 0.22 μm of organic filter membrane, obtain the matrix matching standard solution of corresponding concentration.
2, sample pre-treatments:
Smashed Tea Samples 1g is weighed in 50mL plastic centrifuge tube, 1g anhydrous sodium sulfate and 15mL n-hexane-the third is added
Ketone (1:1, v/v) solution is vortexed and mixes, and ultrasonic extraction 15min, 8000r/min centrifugation 4min takes supernatant to teat glass
In, nitrogen blows concentration, is then settled to 5mL with toluene, to be clean.
0.15g modified carbon nano-tube and 0.15g PSA and 0.1g anhydrous magnesium sulfate are added into solution to be clean, is vortexed,
It is centrifuged 5min with 9000r/min, takes supernatant liquid nitrogen to blow close dry, is quantitatively adding 0.5~1mL n-hexane, is vortexed and mixes, cross 0.22 μ
M organic film is analyzed for GC-MS.
3, instrument operating condition
Chromatographic condition: HP-5MS quartz capillary column (30m × 0.32mm, 0.25 μm)；250 DEG C of injector temperature；Carrier gas is height
Pure nitrogen gas；Flow velocity 1.2mL/min；Splitless injecting samples；1.0 μ L of sample volume.Temperature program: 80 DEG C of initial temperature, 2min is kept；With
20 DEG C/min rate is warming up to 180 DEG C, keeps 2min；230 DEG C are warming up to 3 DEG C/min rate again, keeps 2min；Again with 10
DEG C/min rate is warming up to 280 DEG C, keep 2min.
Mass Spectrometry Conditions: electron bombardment (EI) ion source, ionization voltage 70eV, 280 DEG C of ion source temperature, quadrupole rod temperature
150 DEG C, 280 DEG C of transmission line temperature.
Key instrument used in the above method and equipment: the 7890B-5977A gas chromatograph-mass spectrometer (GC-MS) (U.S.
Agilent company)；KQ-500DE ultrasonic cleaner (Kunshan ultrasonic instrument company)；TG16-WS table model high speed centrifuge (lake
Nan Xiangyi laboratory apparatus company)；K600 pulverizer (German Bo Lang company).
Drug used in the above method and reagent: 18 kinds of PCBs mixed standard solutions, mass concentration are that 10mg/L (is purchased from
O2si company, the U.S.).Modified carbon nano-tube (length: 10~30 μm, outer diameter: 10~20nm, internal diameter: 5~10nm, purity: >
95%, specific surface area: > 200m2/ g), it is purchased from Nanjing Xian Feng Nono-material Science & Technology Ltd.；Acetone, ethyl acetate, acetonitrile,
Sodium chloride, anhydrous sodium sulfate (with the preceding calcination 4h at 450 DEG C), anhydrous magnesium sulfate (with the preceding calcination 4h at 620 DEG C), are point
Analyse pure (Shanghai Chinese medicines group company).
The test result of the present embodiment:
1, chromatographic mass spectrometry separates
Table 1 and attached drawing 1 are respectively the chromatographic mass spectrometry information and separating effect figure of 18 kinds of PCBs, and * indicates quota ion in table 1.It can
See, 18 kinds of PCBs separating degrees are good, and appearance is compact and peak shape is symmetrical, and analytical cycle ensure that separating effect less than 30 minutes
While, realize the purpose and effect quickly analyzed.
Retention time, characteristic ion and its relative abundance of 1 18 kinds of PCBs of table
2, the range of linearity and lower limit of quantitation of method
It prepares the extraction standard working solution that mass concentration is 0.005~0.5mg/kg respectively to be measured, with the peak of object
Area (y) is ordinate, and mass concentration (x) is abscissa, carries out linear regression, draws extraction standard curve.The result shows that
In 0.005~0.5mg/kg concentration range, each object peak area and its concentration are linearly related, and related coefficient (r) is
0.9998~1.0000 (table 2).In a manner of it can accurately measure the minimum additive amount of bare substrate, quantifying for 18 kinds of objects is determined
Lower limit (LOQ) is 0.005mg/kg.
Extraction standard curve, the related coefficient of 2 18 kinds of PCBs of table
3, the rate of recovery and precision of method
In 3 kinds of Biluochun tea, extra-strong tea and Pu'er tea blank tealeaves matrix, the mixed of 0.005~0.1mg/kg is added respectively
Standard liquid is closed, is stood after mixing and obtains mark-on sample, pre-treatment is carried out and measurement, each concentration level is repeated 5 times, calculate the rate of recovery
With relative standard deviation (RSD).The results show that the average recovery rate of each object exists under 3 concentration pitch-based spheres
Between 90.7%~115.2%, RSD is 0.3%~10.9% (table 3).The accuracy of method is high, precision is good.
3 18 kinds of PCBs of table grow tea average recovery rate and relative standard deviation (n=5) in phyllopodium matter 3
4, interpretation of result: the method for the present embodiment effectively reduces the impurity such as pigment in matrix and interferes, and obtains and preferably mentions
Efficiency and clean-up effect are taken, methodology Verification is good, and each object is linear related within the scope of 0.005~0.5mg/kg
(r >=0.9998), for matrix recovery of standard addition between 90.7%~115.2%, RSD (n=5) is equal no more than 10.9%, LOQ
For 0.005mg/kg.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (4)
1. a kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves, it is characterised in that: successively include following
Step:
The first step weighs smashed Tea Samples in centrifuge tube, and anhydrous sodium sulfate and n-hexane-acetone soln is added, according to
It is secondary to carry out vortex mixing, ultrasonic extraction, centrifugation, then take supernatant into test tube, nitrogen blows concentration, is then settled to institute with toluene
Volume is needed, Tea Samples solution to be clean is obtained；Wherein, the mass ratio of the Tea Samples and anhydrous sodium sulfate is 1:1, tealeaves
The input ratio of sample and the n-hexane-acetone soln is that investment 10 ~ 20ml n-hexane-acetone is molten into every 1g fresh tea leaves sample
Liquid；
Modified carbon nano-tube, PSA and anhydrous magnesium sulfate are added into Tea Samples solution to be clean for second step, are vortexed, from
The heart takes supernatant liquid nitrogen to blow close dry, is quantitatively adding n-hexane, is vortexed and mixes, cross organic system filter membrane, obtain Tea Samples scavenging solution,
It is analyzed for GC-MS；Wherein, the modified carbon nano-tube is functionalized multi-wall carbonnanotubes, the Tea Samples, modified carbon nano tube
The mass ratio of pipe, PSA and anhydrous magnesium sulfate is 10:1 ~ 1.5:1 ~ 1.5:1.
2. a kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves according to claim 1, special
Sign is: the volume ratio of n-hexane and acetone is 1:1 in the n-hexane-acetone soln.
3. a kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves according to claim 1, special
Sign is: in the first step, 10 ~ 20min of ultrasonic extraction is centrifuged 2 ~ 8 min with 6000 ~ 9000 r/min.
4. a kind of quick sample pretreatment method detected for Polychlorinated biphenyls in tealeaves according to claim 1, special
Sign is: in the second step, being centrifuged 2 ~ 10 min with 7000 ~ 10000 r/min.
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Cited By (3)
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| CN110243955A (en) * | 2019-05-20 | 2019-09-17 | 兰韬 | It is exclusively used in the QuEChERS purification pipe and application method of interference component in removal tealeaves and tobacco leaf |
| CN110743504A (en) * | 2019-11-15 | 2020-02-04 | 山东农业大学 | Purifying and adsorbing material and application thereof in simultaneous detection of ten pesticide residues in tomatoes |
| CN111458424A (en) * | 2020-03-24 | 2020-07-28 | 东莞市中鼎检测技术有限公司 | Method for detecting tetradecyl chlorotetramethylene in plastic |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110743504A (en) * | 2019-11-15 | 2020-02-04 | 山东农业大学 | Purifying and adsorbing material and application thereof in simultaneous detection of ten pesticide residues in tomatoes |
| CN111458424A (en) * | 2020-03-24 | 2020-07-28 | 东莞市中鼎检测技术有限公司 | Method for detecting tetradecyl chlorotetramethylene in plastic |
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