CN104569244B - The construction method of the liquid-phase chromatograph finger print atlas of essence spice for cigarette - Google Patents
The construction method of the liquid-phase chromatograph finger print atlas of essence spice for cigarette Download PDFInfo
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Abstract
The invention discloses the construction method of the liquid-phase chromatograph finger print atlas of a kind of essence spice for cigarette.Being that the analysis utilizing the diode array detector of liquid chromatograph and refractive index detector to carry out liquid-phase chromatograph finger print atlas builds, the Parameter Conditions of described liquid chromatograph is: chromatographic column: METACARB H PLUS 300 × 7.8 mm；Guard column: METACARB H PLUS guard column；Column oven temperature: 60 DEG C；Flowing phase: 6 mM H2SO4；Flow velocity: 0.4 mL/min；The termination of pumping time: 120 min.The present invention studies for a long period of time based on to essence spice for cigarette substance characteristics, diode array detector and the refractive index detector of scientific utilization liquid chromatograph are combined, specific aim sums up accurate analysis condition, realize the structure of the liquid-phase chromatograph finger print atlas of essence spice for cigarette, reflect the fingerprint characteristic of essence spice for cigarette sample comprehensively, the fingerprint map construction of the essence spice for cigarette samples such as sugary, sugar alcohol can be efficiently applied to, have bigger actual application value.
Description
Technical field
The invention belongs to Analysis of Tobacco Flavor detection and Quality Control Technology field, more particularly, to the construction method of the liquid-phase chromatograph finger print atlas of a kind of essence spice for cigarette.
Background technology
Essence spice for cigarette technology is one of important core technology of tobacco business, and the essence spice for cigarette aromatic style feature to keeping cigarette brand is significant.The change of essence and flavoring agent quality directly affects the quality of Medicated cigarette.Essence spice for cigarette has drawn from natural perfume material more, its quality can be affected by the factors such as original producton location, production technology, and essence spice for cigarette comes from the synergism between self Multiple components to the impact of cigarette quality, so the analytical chemistry composition of system, the finger printing setting up reflection ingredient comprehensively will more efficiently embody the globality of its chemical composition.Qualitatively the quality of essence spice for cigarette to be monitored by calculating similarity between finger printing, be a kind of important and preferable controlling soil moist.The finger printing applying liquid chromatograph to set up essence and flavoring agent can be effectively applied to safety and all many-sides such as quality stability control and character distinction of essence spice for cigarette, has great importance.The multiformity of the chemical composition of essence spice for cigarette and complexity always are emphasis and the difficult point of its quality control, the acquisition of essence spice for cigarette finger printing, only could stablize after setting up the liquid phase chromatography analytical method of science, easy and effectively obtain.
A kind of technology studying complex material system on the whole that finger printing is as modern analytical technique development and is born, is applied at present in the fields such as environmental conservation, food evaluation, Chinese medicine quality control, and especially on Chinese crude drug, Application comparison is extensive.And application report that finger printing is in terms of quality of flavoring essence for tobacco control is relatively fewer.
Existing research has the combination utilizing gas chromatogram-GC-MS (GC/MS) two kinds of analytical tool to be analyzed the chemical composition of essence spice for cigarette, obtain the finger printing of feature, by calculating the numerical value of fingerprint similarity between actual measurement sample and standard sample, it is judged that the degree of closeness of both intrinsic chemical compositions.
High performance liquid chromatography is one of very important analysis method, uses wide at tobacco productive corporation and research unit.Along with Product checking requirement is improved constantly, HPLC uses detector multiple techniques, has made some progress, but majority is at the field of Chinese medicines.But current rare application high performance liquid chromatography carries out the finger printing research of essence spice for cigarette.Because in making a concrete analysis of specific object, select what kind of detector to carry out being combined, how to carry out the connection between detector, sample should the most scientifically pretreatment, in the case of described detector is combined, how to determine that the aspects such as concrete testing conditions also exist a lot of rucial scientific and technological problems and need to go to capture, as a example by chromatographic column, chromatographic column expensive, if carrying out simple screening process conditions with reference to existing achievement in research, constantly replacing chromatographic column is to obtain final scheme, and expensive research cost is difficult to bear.And interact between each process conditions, check and balance, lower cost how can be used to go to carry out more effectively, analyze work efficiently, always annoying the technical barrier of the art, it is combined achievement in research for the detector acquired by a kind of object and can not be applied to another kind of object referring briefly to ground, in particular for chemical composition, there is multiformity and the essence spice for cigarette of complexity feature.
Have no at present and two kinds of detector science combinations realize single injected sampling success and combines suitable chromatographic separation condition being successfully established the correlation technique report of essence spice for cigarette finger printing.
Summary of the invention
The present invention to solve the technical problem that the technical deficiency being to set up essence spice for cigarette finger printing for existing application liquid chromatograph, it is provided that the construction method of the liquid-phase chromatograph finger print atlas of a kind of essence spice for cigarette.
Another of the present invention to solve the technical problem that the application being to provide described construction method.
The purpose of the present invention is achieved by the following technical programs:
The construction method of the liquid-phase chromatograph finger print atlas of a kind of essence spice for cigarette is provided, being that the analysis utilizing the diode array detector (PDAD) of liquid chromatograph and refractive index detector (RID) to carry out liquid-phase chromatograph finger print atlas builds, the Parameter Conditions of described liquid chromatograph is:
Chromatographic column: METACARB H PLUS 300 × 7.8 mm；
Guard column: METACARB H PLUS guard column；
Column oven temperature: 60 DEG C；
Flowing phase: 6 mM H2SO4；
Flow velocity: 0.4 mL/min；
The termination of pumping time: 120 min.
Diode array detector detection wavelength: 200～360 nm；
Refractive index detector optical element temperature: 30～45 DEG C.
It is further preferred that described DAD detection wavelength: 210 nm；
It is further preferred that described RID optical element temperature: 35 DEG C.
The construction method of the liquid-phase chromatograph finger print atlas of described essence spice for cigarette, uses simple same procedure to realize single injected sampling after sample is carried out pre-treatment, obtains the fingerprint map analyzing of tobacco sample comprehensively.Said method comprising the steps of:
S1. sample pre-treatments；
S2. device builds；Being installed in liquid chromatograph instrument by two kinds of detectors, wherein diode array detector is front, and refractive index detector is rear；Flowing phase liquid first passes through diode array detector, then through refractive index detector, finally discharges detector as waste liquid；
S3. sample introduction analysis；
Wherein, the sample pre-treatments described in S1 specifically takes 0.1 mL sample and is placed in 10 mL volumetric flasks, with 6 mM H2SO4Filter after constant volume mixing.
Preferably, described filtration is to filter through 0.45 μm nylon leaching film.
Preferably, the amount of described sample introduction is 10 μ L.
Present invention simultaneously provides the application of described construction method, be applied to set up the finger printing of essence spice for cigarette sample.It is applied especially to the fingerprint map construction of the essence spice for cigarette sample of sugary and/or sugar alcohol.
Beneficial effects of the present invention is embodied in:
Diode array detector (PDAD) is a kind of optical multichannel detectors just occurred the eighties in 20th century, and it can be regarded as a branch of UVD, is applied to the qualitative and quantitative analysis of biological sample, Chinese herbal medicine at present.The sensitivity of diode array detector (PDAD) is preferable, but the applicant studies discovery, diode array detector (PDAD) has deficiency at analysis essence spice for cigarette, the compound without ultraviolet absorption group is not responded to, and much essence spice for cigarette all contains this compounds (such as sugar or sugar alcohols), the most individually use diode array detector (PDAD) that sugar or the Fingerprints of sugar alcohols compound cannot be embodied, differential refraction detector (RID) is a kind of common detector, as long as tested component has difference just can use with the refraction index of eluent.The sensitivity of differential refraction detector (RID) is relatively low, but has preferably response to the material not having uv absorption, the most easily uses simultaneously, and maintenance cost is low.The applicant's creatively research summary finds the fingerprint map analyzing utilizing the combination of diode array detector and differential refraction detector to realize essence spice for cigarette.
But in actual applications, owing to essence spice for cigarette chemical composition has multiformity and complexity feature, the combination design being based only on diode array detector and differential refraction detector can not realize the fingerprint map analyzing of sample smoothly.The combination design of diode array detector and differential refraction detector must rationally, systematically be combined the fingerprint map analyzing that could successfully solve essence spice for cigarette with the sample-pretreating method of science, chromatographic isolation overall technical architecture.
Based on the applicant, the long-term specific aim of essence spice for cigarette substance characteristics is furtherd investigate, sum up the H using concentration to be 6 mM2SO4Make an addition in proportion sample uses after constant volume 0.45 μm nylon leaching film to filter the sample liquid obtained to can be used for single injected sampling and ensure being successfully completed of follow-up separation and fingerprint map analyzing to carrying out dissolving.
Further, the present invention uses METACARB H PLUS 300 × 7.8
Mm is as chromatographic column and uses METACARB H PLUS guard column simultaneously; research for matching sums up suitable Split liquid chromatographic apparatus and accurate technique; obtain and be preferably applicable to separating effect associated with the two detector, finally realize row combination in conjunction with the suitable combination mode of diode array detector (DAD) and refractive index detector (RID).
Further, the present invention combine science sample-pretreating method obtain sample introduction sample liquid, it is achieved single injected sampling, be successfully separated and realize two kinds of detectors associating finger printing output.
In sum, the invention provides a kind of system complete, fingerprint map construction method for essence spice for cigarette, from the sample-pretreating method of science, obtain research for matching and sum up suitable Split liquid chromatographic apparatus and accurate technique, obtain and be preferably applicable to separating effect associated with the two detector, mode properly it is combined in conjunction with diode array detector (DAD) and refractive index detector (RID), obtain the finger printing information of essence spice for cigarette conveniently and efficiently, the fingerprint characteristic of essence spice for cigarette sample can be highlighted, the fingerprint map construction containing the essence spice for cigarette sample without ultraviolet absorption group compound can be efficiently applied to, there is important actual application value.
Accompanying drawing explanation
Fig. 1 embodiment 1 finger printing.
Fig. 2 embodiment 1 finger printing partial enlarged drawing.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the accompanying drawings with specific embodiment.Unless stated otherwise, the embodiment of the present invention uses equipment, reagent and method are equipment, reagent and method commonly used in the art.
Embodiment 1
The present embodiment uses Agilent 1200 chromatograph of liquid, joins DAD and RID；Concentrated sulphuric acid (analytical pure), ultra-pure water；0.45 μm nylon leaching film.Thering is provided by Guangdong China Tobacco Industry Co., Ltd for detecting the essence spice for cigarette sample of analysis, sample is merely to illustrate the inventive method, the most therefore limits the sample scope that the inventive method is suitable for.
Prepare 6 mM H2SO4Solution (compound method is conventional with reference to this area).
Detection analytical procedure is as follows:
S1. sample pre-treatments: take 0.1 mL essence spice for cigarette sample and be placed in 10 mL volumetric flasks, with 6 mM H2SO4Constant volume also mixes, in case subsequent step carries out liquid-phase chromatographic analysis after 0.45 μm nylon leaching film filters；
S2. device builds；Being installed in liquid chromatograph instrument by two kinds of detectors, wherein diode array detector is front, and refractive index detector is rear；Flowing phase liquid first passes through diode array detector, then through refractive index detector, finally discharges detector as waste liquid；
S3. sample introduction analysis；
The present embodiment sample introduction measures 10 μ L.
In experimentation, the present embodiment simultaneously primary study changes DAD and detects the wavelength impact on testing result, and after changing wavelength, the peak height of the chromatographic peak in DAD chromatogram can decrease, i.e. detection sensitivity can decrease.The raising of sensitivity, is conducive to obtaining more profile information.Experiment finds in the case of other testing conditions of the present invention are certain, it is provided that wavelength in 200～360 nm wave-length coverages, be suitable for analyzing multiple compounds, can fully obtain the finger printing information of essence spice for cigarette.The present embodiment simultaneously primary study change RID optical element temperature is tested.Experiment finds, RID optical element temperature is arranged in the range of 30～45 DEG C, and the impact on RID chromatogram is inconspicuous, basically identical with artwork.
The factors such as the specific aim of Considering experimental object, the accuracy of experimental result, sensitivity, the analytical parameters condition of the optimum liquid chromatograph finally determined is:
Chromatographic column: METACARB H PLUS 300 × 7.8 mm；
Guard column: METACARB H PLUS guard column；
Column oven temperature: 60 DEG C；
Flowing phase: 6 mM H2SO4；
Flow velocity: 0.4 mL/min；
The termination of pumping time: 120 min；
DAD detects wavelength: 210 nM；
RID optical element temperature: 35 DEG C.
Under above-mentioned analysis condition, it is thus achieved that finger printing is asked for an interview shown in accompanying drawing 1, upper figure is DAD chromatogram, and figure below is RID chromatogram.Accompanying drawing 2 is the finger printing of partial enlargement.Having accompanying drawing visible, the present invention sums up the structure that scientific and reasonable pre-treatment side realizes the liquid-phase chromatograph finger print atlas of essence spice for cigarette.From finger printing, this sample composition is fairly simple, is substantially free of sugar or sugar alcohols material, and analysis result is consistent with other conventional method testing results.The component colony analysis chart spectrum of the essence sample for tobacco Chemical Characteristics obtained based on the present embodiment combines conventional computational analysis technology to sample can carry out exclusive, macroscopical, overall chemical feature integrated information analytical calculation research.
Claims (5)
1. the construction method of the liquid-phase chromatograph finger print atlas of an essence spice for cigarette, it is characterised in that be to utilize
The diode array detector of liquid chromatograph and refractive index detector carry out the analysis of liquid-phase chromatograph finger print atlas
Building, the Parameter Conditions of described liquid chromatograph is:
Chromatographic column: METACARB H PLUS 300 × 7.8mm；
Guard column: METACARB H PLUS guard column；
Column oven temperature: 60 DEG C；
Flowing phase: 6mM H2SO4；
Flow velocity: 0.4mL/min；
Termination of pumping time: 120min；
Diode array detector detection wavelength: 210nm；
Refractive index detector optical element temperature: 35 DEG C；
The construction method of the liquid-phase chromatograph finger print atlas of described essence spice for cigarette comprises the following steps:
S1. sample pre-treatments；
S2. device builds；Two kinds of detectors are installed in liquid chromatograph instrument, wherein photodiode array detection
Device is front, and refractive index detector is rear；Flowing phase liquid first passes through diode array detector, then through folding
Optical index detector, finally discharges detector as waste liquid；
S3. sample introduction analysis；
Wherein, the sample pre-treatments described in S1 specifically takes 0.1mL sample and is placed in 10mL volumetric flask, with 6
mM H2SO4Filter after constant volume mixing.
The most according to claim 1, the construction method of the liquid-phase chromatograph finger print atlas of essence spice for cigarette, it is special
Levying and be, described filtration is to filter through 0.45 μm nylon leaching film.
The most according to claim 1, the construction method of the liquid-phase chromatograph finger print atlas of essence spice for cigarette, it is special
Levying and be, the amount of described sample introduction is 10 μ L.
4. the application of construction method described in claim 1,2 or 3, it is characterised in that be applied to set up cigarette and use
The finger printing of essence and flavoring agent sample.
5. the application of construction method described in claim 4, it is characterised in that be applied to the sugary and/or cigarette of sugar alcohol
Fingerprint map construction with essence and flavoring agent sample.
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| CN106404877B (en) * | 2016-08-19 | 2019-05-03 | 陕西中烟工业有限责任公司 | Flavors and fragrances Fourier Transform Ion cyclotron Resonance mass spectrum fingerprint pattern analysis method |
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| CA2772131A1 (en) * | 2009-08-31 | 2011-03-03 | Iogen Energy Corporation | Fermentation method to produce a lignocellulose-based sugar stream with enriched pentose content |
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| CN101566607A (en) * | 2009-06-03 | 2009-10-28 | 川渝中烟工业公司 | Method for measuring organic acid radicals in cigarette paper |
| CN102520094A (en) * | 2011-12-28 | 2012-06-27 | 广东中烟工业有限责任公司 | Method for determining glucose, fructose and saccharose in tobacco essence perfume |
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