CN103399104B - Pretreatment kit for detecting phthalic acid ester in tea and treatment method of pretreatment kit - Google Patents
Pretreatment kit for detecting phthalic acid ester in tea and treatment method of pretreatment kit Download PDFInfo
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- CN103399104B CN103399104B CN201310328282.3A CN201310328282A CN103399104B CN 103399104 B CN103399104 B CN 103399104B CN 201310328282 A CN201310328282 A CN 201310328282A CN 103399104 B CN103399104 B CN 103399104B
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Abstract
The invention discloses a pretreatment kit for detecting phthalic acid ester in tea and belongs to the technical field of chemical analysis methods. The kit comprises a kit pipe 1 and a kit pipe 2, wherein the kit pipe 1 contains 4-6g of sodium chloride, and the kit pipe 2 contains 80-100mg of graphitized carbon black, 150-200mg of N-propylethylenediamine and 80-120mg of calcium chloride. The kit is reasonable in design and does not adopt plastic products, so that the background pollution introduced by a test ware is avoided and the pollution resistance of a detection method is improved; when the kit is utilized for treatment, the steps of solvent replacement, concentration and the like are avoided, not only is the background pollution introduced in the operation process reduced, but also the operation is simple, the operation time of the whole process is shorter than 60 minutes and the working efficiency is improved; an organic solvent needed in treatment is only acetonitrile, so that the cost is saved, and the use of toxic and harmful reagents is reduced.
Description
Technical field
The invention belongs to chemical analysis method technical field, be specifically related to phthalic ester in a kind of tealeaves and detect pretreatment reagent kit and disposal route thereof.
Background technology
Phthalic ester is the endocrine disruption hormone paid close attention in the world, huge to the reproductive development harm of human body, also has cardiac toxic, hepatotoxicity wind agitation and renal toxicity simultaneously.Phthalic ester is mainly used as plastifier, is widely used in plastic package material.Plastics package is the principal mode of tea packaging, especially low and middle-grade tealeaves.Plastics package adopts coloured picture case to make attractive packages mostly, and also often containing phthalic ester in these color pigments.Therefore, the phthalic ester in tea packaging and colour-wash very likely migrates to tealeaves, harm consumer health.The experimental results shows, tealeaves detects the phthalic esters such as DiBP, DBP, DEHP.
Phthalic ester detection method mainly comprises pretreatment technology and instrument analysis technology.Pre-treatment step mainly comprises: target compound is through Solvent Extract methods such as acetonitrile, acetone, normal hexanes, then adopt the technology such as liquid-liquid extraction, Solid-Phase Extraction or gel purification chromatogram to purify extract, remove or reduce the interference that sample substrate detects phthalic ester.In pretreatment process, extracting and purifying is the most key step, and different Extraction solvent is different to the extraction efficiency of phthalic ester in tealeaves with extracting mode, causes detection method to occur deviation; There is bigger difference in the removal effect of different purification styles to interference impurity, the existence of interfering material causes qualitative, quantitative deviation.The main application of phthalic ester is softening function, is widely used in plastic products, increases the plasticity of goods.Therefore, use the plastic products such as plastic centrifuge tube, liquid-transfering gun, solid phase extraction column (shell is plastic products), the organic filter membrane of PVC all may introduce phthalic ester in pre-treatment, we carry out detection to above-mentioned pre-treatment material and find, these plastic products all contain phthalic ester in various degree, cause severe jamming to detection method.Meanwhile, too much operation steps can increase the risk that in pretreatment process, phthalic ester is introduced, and as steps such as solvent displacement, liquid concentration, thus causes method false positive or quantitative deviation.In China's national standard and industry standard, the pretreatment technology that in solid sample, phthalic ester detects adopts the organic reagents such as normal hexane, ethyl acetate, acetonitrile to extract usually, liquid-liquid extraction or Solid phase extraction.There is the shortcomings such as complicated operation, solvent consumption are large, time-consuming in these pretreatment technologies, is difficult to avoid pretreatment process to introduce the cross pollution of phthalic ester; Meanwhile, adopt the plastic products such as Solid phase extraction pillar, organic filter membrane in China's phthalic ester detection method part of standards, this is all the source of phthalic ester background interference, causes testing result inaccurate.Large quantity research has been carried out to phthalic ester detection method both at home and abroad, but in existing tealeaves, phthalic ester detects pretreatment technology and there is the shortcoming of contamination resistance difference, and complicated operation, time-consuming, solvent consumption is large.
Summary of the invention
For prior art Problems existing, the object of the invention is to design provides phthalic ester in a kind of tealeaves to detect the technical scheme of pretreatment reagent kit and disposal route thereof.
In described a kind of tealeaves, phthalic ester detects pretreatment reagent kit, it is characterized in that in described kit pipe 2 containing 85 ~ 95 mg Graphons, 160 ~ 180mg N-propyl group ethylenediamine and 90 ~ 110 mg lime chloride.
In described a kind of tealeaves, phthalic ester detects pretreatment reagent kit, it is characterized in that comprising kit pipe 1 and kit pipe 2, containing 4 ~ 6 g sodium chloride in described kit pipe 1, containing 80 ~ 100 mg Graphons, 150 ~ 200 mg N-propyl group ethylenediamines and 80 ~ 120 mg lime chloride in described kit pipe 2.
In described a kind of tealeaves, phthalic ester detects pretreatment reagent kit, it is characterized in that described kit pipe 1 and kit pipe 2 are ground tool plug glass centrifuge tube.
In described a kind of tealeaves, phthalic ester detects the disposal route of pretreatment reagent kit, it is characterized in that comprising the following steps:
1) taking dry tea powder 2 g joins in kit pipe 1, add deionized water, 10 ~ 15min is left standstill after hand 1 ~ 2min, 10ml trifluoroacetic acid aqueous solution is added again in kit pipe 1, then 2 min are extracted with 10000 ~ 12000 r/min homogeneous, hand 0.5 ~ 1 min, through centrifugal 10 ~ 12 min of 4000 ~ 6000 r/min;
2) getting with glass pipet the upper liquid 2mL that step 1) obtains and join kit pipe 2, handly acutely rock 1 min, through centrifugal 10 ~ 12 min of 4000 ~ 6000 r/min, then getting upper liquid for analyzing.
In above-mentioned a kind of tealeaves, phthalic ester detects pretreatment reagent kit, reasonable in design, does not adopt plastic products, thus avoids the background contamination introduced by tester, improve the contamination resistance of detection method in this kit; When utilizing this kit to process, solvent-free displacement, the step such as concentrated, not only reduce the background contamination introduced in operating process, and simple to operate, and the whole process operation time is less than 60 min, improves work efficiency; Organic solvent required during process only has acetonitrile, has saved cost, reduces the use of poisonous and harmful reagent.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1: concrete operation method
Get the dry tea of 50-100 g through pulverizer grinds, take 2.0 g with the electronic balance of sensibility reciprocal 0.0001g and join kit pipe 1,5 mL deionized waters are added again with glass pipet, hand 1,1.5 or 2min after leave standstill 10,12 or 15min, 10 mL trifluoroacetic acid aqueous solution are added again in pipe 1, extract 2 min with 10000,11000 or 12000 r/min homogeneous, handly acutely rock 0.5,0.8 or 1min, centrifuge tube is through 4000,5000 or centrifugal 10,11 or 12 min of 6000r/min; Get upper liquid 2 mL with glass pipet and join kit pipe 2, handly acutely rock 1min, through centrifugal 10,11 or 12 min of 4000,5000 or 6000 r/min, get upper liquid 1-1.5 mL in the gas chromatography tandem mass spectrometry auto injection bottle of 1.5 mL.
Containing 5g sodium chloride in kit pipe 1, containing 90 mg Graphons, 180mg N-propyl group ethylenediamine and 100mg lime chloride in kit pipe 2; Or adopt containing 4g sodium chloride in kit pipe 1, containing 80 mg Graphons, 150 mg N-propyl group ethylenediamines and 80 mg lime chloride in kit pipe 2; Or adopt containing 6 g sodium chloride in kit pipe 1, containing 100 mg Graphons, 200 mg N-propyl group ethylenediamines and 120 mg lime chloride in kit pipe 2.Kit pipe 1 and kit pipe 2 are ground tool plug glass centrifuge tube.
Gas chromatography tandem mass spectrometry testing conditions is:
Mm × 0.25 μm, VF-5MS capillary column 30 m × 0.25, carrier gas is high-purity helium (99.999%), flow velocity 1.0 mL/min.Column temperature initial temperature 80 DEG C, keeps 1 min, with 15 DEG C/min ramp to 180 DEG C, retains 2 min, keeps 0.33 min with 5 DEG C/min ramp to 280 DEG C.Input mode, for not shunt, opens diverting valve after 0.75 min, sample size 1 μ L, injector temperature 220 DEG C, connecting link temperature 280 DEG C.
Ionization mode is electron impact ionization source (EI), ionizing energy 70 eV, filament current 50 mA, EMV voltage 1 000 V.Quadrupole rod temperature 40 DEG C, ion source temperature 230 DEG C, solvent delay 5 min.Collision gas is high-purity argon gas (99.999%), collision atmospheric pressure 2 mTor.The MRM parameters such as 7 kinds of target analytes ion pairs, collision voltages are in Table following table.
Embodiment 2: different tealeaves matrix clean-up effect
After adopting the extract of pretreatment reagent kit of the present invention to black tea (BT) and green tea (GT) to carry out pre-treatment according to the step of embodiment 1, handle well, the initial extraction liquid of black tea and green tea becomes light yellow clear shape by original aterrimus, and Tea Polyphenols declines more than 50%, caffeine declines 15%.
Conclusion: this embodiment 2 illustrates and adopts pretreatment reagent kit of the present invention can effectively remove tealeaves interfering material, improves accuracy and the precision of detection method, and reduces instrument loss.
Embodiment 3: quality-control sample is tested
Carry out recovery test at 0.1 mg/kg and 0.5 mg/kg level, the recovery of 8 kinds of phthalic esters is:
8 kinds of typical phthalic ester recovery of standard addition
Conclusion: this embodiment 3 illustrates that Tea Samples extracts through pretreatment reagent kit of the present invention and after purification, detection method accuracy is high, reproducible, meets phthalic ester testing requirement in tealeaves.
Embodiment 4: phthalic ester residues detection in actual sample
Adopt China's standard GB/T/T 23204-2008 recommend method and pretreatment reagent kit of the present invention to test Tea Samples, and blank solvent contrast be set, the results are shown in following table:
The content (unit mg/kg) of phthalic ester in blank solvent and tealeaves
Conclusion: this embodiment 4 illustrates that pretreatment reagent kit anti-jamming effectiveness of the present invention is significantly higher than Solid-Phase Extraction pre-treating method.
Claims (2)
1. in a tealeaves, phthalic ester detects pretreatment reagent kit, it is characterized in that comprising kit pipe 1 and kit pipe 2, containing 4 ~ 6 g sodium chloride in described kit pipe 1, containing 85 ~ 95mg Graphon, 160 ~ 180mg N-propyl group ethylenediamine and 90 ~ 110 mg lime chloride in described kit pipe 2;
Utilize phthalic ester in this tealeaves to detect the disposal route of pretreatment reagent kit, comprise the following steps:
1) taking dry tea powder 2 g joins in kit pipe 1, add deionized water, 10 ~ 15 min are left standstill after hand 1 ~ 2 min, 10 ml trifluoroacetic acid aqueous solution are added again in kit pipe 1, then 2min is extracted with 10000 ~ 12000 r/min homogeneous, hand 0.5 ~ 1 min, through centrifugal 10 ~ 12 min of 4000 ~ 6000 r/min;
2) getting with glass pipet the upper liquid 2mL that step 1) obtains and join kit pipe 2, handly acutely rock 1min, through centrifugal 10 ~ 12 min of 4000 ~ 6000 r/min, then getting upper liquid for analyzing.
2. in a kind of tealeaves as claimed in claim 1, phthalic ester detects pretreatment reagent kit, it is characterized in that described kit pipe 1 and kit pipe 2 are ground tool plug glass centrifuge tube.
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| CN201310328282.3A CN103399104B (en) | 2013-07-31 | 2013-07-31 | Pretreatment kit for detecting phthalic acid ester in tea and treatment method of pretreatment kit |
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| CN108008029B (en) * | 2017-11-13 | 2020-09-22 | 浙江省海洋水产研究所 | Dispersed solid phase extraction-gas chromatography-mass spectrometry detection method for phthalate ester environmental hormone in marine sediment |
| CN108008028B (en) * | 2017-11-13 | 2020-08-14 | 浙江省海洋水产研究所 | Dispersed solid phase extraction-gas chromatography-mass spectrometry detection method for phthalate ester environmental hormone in marine products |
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