CN103868980A - Application of doping agent in test of phthalic acid ester compounds by use of ion mobility spectrometry - Google Patents
Application of doping agent in test of phthalic acid ester compounds by use of ion mobility spectrometry Download PDFInfo
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- CN103868980A CN103868980A CN201210539684.3A CN201210539684A CN103868980A CN 103868980 A CN103868980 A CN 103868980A CN 201210539684 A CN201210539684 A CN 201210539684A CN 103868980 A CN103868980 A CN 103868980A
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- adulterant
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Abstract
The invention relates to a method for rapid and sensitive test of phthalic acid ester compounds. An ion mobility spectrometry technology using a radioactive source as an ionization source is used as a basic test technology, and in the positive ion mode, a doping agent is added into a circulation gas path to establish the method for test of the phthalic acid ester compounds. Background spectrum peaks of an ion mobility spectrum in the positive ion mode can be purified by addition of the doping agent, and selectivity and sensitivity of the test of the phthalic acid ester compounds can be improved.
Description
Technical field
The present invention relates to one and realize phthalate compound high selectivity, highly sensitive detection method.The method, take the ion mobility spectrometry in radioactive ionization gauge source as basic detection technique, under positive ion mode, by add volatile adulterant in circulation gas circuit, is set up phthalate compound high selectivity, highly sensitive detection method.The method realizes selective reaction by the proton affinity of adulterant, has purified the background spectra peak under ion mobility spectrometry positive ion mode, has improved selectivity and sensitivity that phthalate compound detects.
Background technology
Phthalic ester is the chemicals that a class can play emollescence, is often used as plastifier and is widely used in toy manufacture, packaging for foodstuff, Medical blood bag and sebific duct, vinyl flooring and wallpaper, detersive, lubricating oil and personal-care supplies.The phthalate the most often adding in plastics comprises phthalic acid and butyl ester (DBP), dioctyl phthalate (DNOP), phthalic acid butyloxy phenyl (BBP), O-phthalic two isodecyl esters (DIDP), diisononyl phthalate (DINP) and phthalic acid two (2-ethylhexyl) ester (DEHP).
Phthalate is a kind of environmental hormone, in human body and animal body, bringing into play the effect of similar female hormone, can disturbance endocrine, mankind spermatozoon quantity is reduced, locomitivity is low, paramophia, serious necrozoospermia and the carcinoma of testis of also can causing is " arch-criminal " who causes male genetic problem.Also there is carcinogenic, teratogenesis, mutagenic effect simultaneously.
Phthalate can enter human body by drinking-water, feed, skin contact and breath light approach, and this compounds has become global main environment organic contaminant.Due to the extensive existence of phthalic ester and the harm to human body, make its detection method be paid close attention to widely.Used detects phthalate compound in textile, food and toy for children by the method for gas chromatography-mass spectrography.But the method wastes time and energy, and cost is higher.
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology is that the one that 20 century 70s occur separates detection technique fast, compared with traditional mass spectrum, chromatographic apparatus, have simple in structure, highly sensitive, analysis speed is fast, the feature of reliable results.Can in atmospheric environment, detect micro substance, be suitable for on-the-spot use.We IMS of research has been widely used in the fields such as chemical warfare agent, drugs, explosive detection, environmental monitoring, monitoring poisonous gas, fire monitoring, water pollution monitoring and Food Monitoring at present.Ion mobility spectrometry is mainly made up of chamber, ion gate, drift region and detecting device.Sample gas produces molecule, ion in chamber ionization.The ion gate that ion is opened by periodicity under the ordering about of electric field enters drift region.With the neutral drift gas molecule of adverse current constantly in the process of collision, due to these ions migration rate difference separately in electric field, different ions is separated, successively arrive collector detected.Therefore just can determine the existence of evaluating objects material by transit time, and application peak area or peak height can be determined the concentration of respective substance.
Summary of the invention
In order to realize phthalic ester environmental hormone compounds high selectivity, highly sensitive detection, the technical solution used in the present invention is:
Adulterant detects the application in phthalate compound at ion mobility spectrometry, adulterant adds in the circulation gas circuit of ion mobility spectrometry, adulterant is due to its higher proton affinity, the reactive ion reaction that can produce with radioactive ionization gauge source, form dopant ion, avoid the interference of the compound that proton affinity is low, realized phthalic ester steroids compound high selectivity, highly sensitive detection.
Wei Nie source, radioactive ionization gauge source or americium ionization source that ion mobility spectrometry adopts.
Selected adulterant is volatile compound, and described adulterant can add in carrier gas gas circuit, float in gas gas circuit or carrier gas and floating in the total gas circuit of gas front end.
Test by ion mobility spectrometry detecting instrument, ion mobility spectrometry positive ion mode can obtain desirable detection signal.
The H that the proton affinity of adulterant should produce higher than radioactive ionization gauge source
+(H
2o)
ndeng reagent ion, but lower than phthalic ester steroids compound.
Between the reagent ion and determinand phthalate compound producing in radioactive ionization gauge source due to the proton affinity of adulterant, it can eliminate the interference of proton affinity lower than the impurity of dopant compound proton affinity, make background spectra peak cleaner, do not affect the detection of phthalic ester steroids compound simultaneously.
Described adulterant be the one in acetone, ethanol or butanone.
The use of adulterant, can improve the selectivity of phthalic ester steroids compound test, has improved the sensitivity detecting.
Selected adulterant addition in gas circuit is the 0.01-0.1 ‰ of gas gross volume in gas circuit.
Adulterant between the present invention produces proton affinity reagent ion between radioactive ionization gauge source and phthalate compound to be detected is added in the circulation gas circuit of ion mobility spectrometry, can avoid the interference of proton affinity lower than the impurity of adulterant, purify the background spectrogram under positive ion mode, improve selectivity and the sensitivity of phthalic ester steroids compound test.
Adulterant adds in the circulation gas circuit of ion mobility spectrometry, can add carrier gas to, floats gas or carrier gas and float in the total gas circuit of gas front end.
Advantage of the present invention is:
1. the effumability compound between the reagent ion that employing proton affinity produces between radioactive ionization gauge source and phthalate compound to be detected is as adulterant, be added in the circulation gas circuit of ion mobility spectrometry, can avoid the interference of proton affinity lower than the impurity of adulterant, purify the background spectrogram under positive ion mode.
2. the use of adulterant, the selectivity and the sensitivity that have improved phthalic ester steroids compound test.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further detailed explanation:
Fig. 1 is the structural representation of adulterant adding set and ion mobility spectrometry;
Fig. 2 is the ion mobility spectrometry figure at ion mobility spectrometry air reagent ion peak (RIP) and the ion mobility spectrometry figure of acetone under positive ion mode;
Fig. 3 is the ion mobility spectrometry detection spectrogram that under positive ion mode, acetone is made five kinds of phthalate compounds of adulterant;
Fig. 4 is that the ion mobility spectrometry that under positive ion mode, acetone is made three kinds of phthalate compounds of adulterant quantitatively detects spectrogram.
Embodiment
It is detecting instrument that this application is utilized the ionic migration spectrometer in the nickel radioactive ionization gauge source of positive ion mode, adopt the proton affinity effumability compound between air reagent ion peak and phthalate compound to be detected to make adulterant, realize the high sensitivity of Phthalates of Environment Hormone compound, the detection of high selectivity.
Fig. 1 is the structural representation of adulterant adding set and ion mobility spectrometry.Ionic migration spectrometer mainly comprises reaction zone 1 and migration area 2.3 is adulterant adding set, the bottle that adulterant reagent is housed is positioned in the head space bottle of a 90ml to the carrier gas 5 head space bottle of flowing through, the reaction zone by the head space steam carrier band of adulterant to ion mobility spectrometry.The reagent ion that doping reagent molecule and air produce in nickel radioactive ionization gauge source 4 and proton affinity form the ion of adulterant lower than the foreign ion reaction of dopant molecule.Dopant ion enters migration area under the pulse action of ion gate 8, arrives Faraday plate 9 detected under the effect of migration area electric field and make-up gas 6.
Fig. 2-4 provide some experiment spectrograms to the present invention give with explanation.The experiment condition of these spectrograms is: when experiment, migration tube temperature remains on 80 ℃, 160 ℃ of injector temperature, carrier gas (air), float gas (air) air-flow and be respectively 400mL/min, 600mL/min, the acetone of 10ppm is added in carrier gas as adulterant.
Get 1-10 μ L, 0.5-100ppm phthalic ester steroids compound solution by sample introduction needle.Under positive ion mode, take ionic migration spectrometer as detecting instrument, carry sample and enter the ionized region of ion mobility spectrometry containing the carrier gas of chemical dopant; Sample is ionized to positive and negative ion in ionized region, and the ion gate of opening by periodicity enters the drift region being made up of uniform electric field, obtains separating and detect in drift region.The mobility constant of different compounds is variant, the speed difference moving in drift region, the asynchronism(-nization) of their arrival detecting devices.Measure time and peak intensity that ion arrives detector, just can confirm classes of compounds, and determine its content according to the signal intensity at peak.
Fig. 2 is the ion mobility spectrometry figure of ion mobility spectrometry air under positive ion mode and the ion mobility spectrometry spectrogram of acetone.As can be seen from the figure, the ion mobility spectrometry figure more complicated of air while not adding acetone in carrier gas, except being positioned at the main peak ion at 11.43ms place, also has other foreign ion to exist; In the time adding acetone make adulterant in carrier gas, mainly form the acetone positive ion peak at 13.54ms place, purify background spectra peak, be conducive to the Measurement accuracy of phthalate compound.
Embodiment 2
Fig. 3 is the ion mobility spectrometry detection spectrogram that acetone is made five kinds of phthalate compounds of adulterant.Do at positive ion mode acetone under the condition of adulterant, repefral forms the characteristic peak that transit time is 15.63ms, diethyl phthalate forms the characteristic peak that migration transit time is 17.41ms, dibutyl phthalate forms the characteristic peak of transit time 21.03ms, dinonyl phthalate forms the characteristic peak of transit time 28.24ms, and didecyl phthalate forms the characteristic peak of transit time 29.45ms.Along with the increase of molecular weight, the transit time of phthalate compound is along with increase, and the method can be identified different types of phthalate compound effectively.
Embodiment 3
Fig. 4 is that the ion mobility spectrometry that under positive ion mode, acetone is made three kinds of phthalate compounds of adulterant quantitatively detects spectrogram.As can be seen from the figure, the method can realize the quantitative detection in 3 magnitudes of phthalate compound, and detectability can reach 50pg.
Claims (9)
1. adulterant detects the application in phthalate compound at ion mobility spectrometry, it is characterized in that:
Adulterant adds in the circulation gas circuit of ion mobility spectrometry, adulterant is due to its higher proton affinity, the reactive ion reaction that can produce with radioactive ionization gauge source, form dopant ion, avoid the interference of the compound that proton affinity is low, realized phthalic ester steroids compound test.
2. method according to claim 1, is characterized in that: Wei Nie source, radioactive ionization gauge source or americium ionization source that ion mobility spectrometry adopts.
3. method according to claim 1, is characterized in that: selected adulterant is volatile compound, and described adulterant can add in carrier gas gas circuit, float in gas gas circuit or carrier gas and floating in the total gas circuit of gas front end.
4. method according to claim 1, is characterized in that: test by ion mobility spectrometry detecting instrument, ion mobility spectrometry positive ion mode can obtain desirable detection signal.
5. method according to claim 1, is characterized in that: the H that the proton affinity of adulterant should produce higher than radioactive ionization gauge source
+(H
2o)
ndeng reagent ion, but lower than phthalic ester steroids compound.
6. method according to claim 5, it is characterized in that: between the reagent ion and determinand phthalate compound producing in radioactive ionization gauge source due to the proton affinity of adulterant, it can eliminate the interference of proton affinity lower than the impurity of dopant compound proton affinity, make background spectra peak cleaner, do not affect the detection of phthalic ester steroids compound simultaneously.
7. according to the method described in claim 1,5 or 6, it is characterized in that: described adulterant be the one in acetone, ethanol or butanone.
8. method according to claim 5, is characterized in that: the use of adulterant, can improve the selectivity of phthalic ester steroids compound test, and improve the sensitivity detecting.
9. according to the method described in claim 1 or 3, it is characterized in that: selected adulterant addition in gas circuit is the 0.01-0.1 ‰ of gas gross volume in gas circuit.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104538276A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Ion source soft ionization device and method under barometric pressure |
| CN106226384A (en) * | 2016-09-22 | 2016-12-14 | 大连工业大学 | A kind of trimethylamine detection method based on Ion mobility spectrometry |
| CN106501346A (en) * | 2016-09-22 | 2017-03-15 | 大连工业大学 | A kind of method of trimethylamine in quick detection aquatic products |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN108088887A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of detection method of front three amine gas |
| CN110632164A (en) * | 2019-10-31 | 2019-12-31 | 大连大学 | Method for simultaneously detecting phthalate compounds in food |
| CN110709009A (en) * | 2017-06-07 | 2020-01-17 | 拉皮斯坎系统股份有限公司 | System and method for substance detection using positive dopants |
| CN111089895A (en) * | 2019-11-29 | 2020-05-01 | 大连大学 | Application of ion mobility spectrometry in rapid detection of phthalate compounds in plastics |
| CN112071738A (en) * | 2019-06-11 | 2020-12-11 | 中国科学院大连化学物理研究所 | Dopant cartridge and method for stably controlling concentration of chemical dopant of ion mobility spectrometry |
| CN112903803A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院大连化学物理研究所 | Device and method for improving detection sensitivity of etomidate blood concentration in operation |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538276A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Ion source soft ionization device and method under barometric pressure |
| CN106226384A (en) * | 2016-09-22 | 2016-12-14 | 大连工业大学 | A kind of trimethylamine detection method based on Ion mobility spectrometry |
| CN106501346A (en) * | 2016-09-22 | 2017-03-15 | 大连工业大学 | A kind of method of trimethylamine in quick detection aquatic products |
| CN106501346B (en) * | 2016-09-22 | 2019-08-13 | 大连工业大学 | A kind of method of trimethylamine in quick detection aquatic products |
| CN106226384B (en) * | 2016-09-22 | 2019-08-13 | 大连工业大学 | A kind of trimethylamine detection method based on Ion mobility spectrometry |
| CN108088887A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of detection method of front three amine gas |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN110709009A (en) * | 2017-06-07 | 2020-01-17 | 拉皮斯坎系统股份有限公司 | System and method for substance detection using positive dopants |
| CN112071738A (en) * | 2019-06-11 | 2020-12-11 | 中国科学院大连化学物理研究所 | Dopant cartridge and method for stably controlling concentration of chemical dopant of ion mobility spectrometry |
| CN110632164A (en) * | 2019-10-31 | 2019-12-31 | 大连大学 | Method for simultaneously detecting phthalate compounds in food |
| CN112903803A (en) * | 2019-11-19 | 2021-06-04 | 中国科学院大连化学物理研究所 | Device and method for improving detection sensitivity of etomidate blood concentration in operation |
| CN111089895A (en) * | 2019-11-29 | 2020-05-01 | 大连大学 | Application of ion mobility spectrometry in rapid detection of phthalate compounds in plastics |
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Application publication date: 20140618 |