CN104451199A - Extraction and purification method and detection method of arsenic form in paper for tobaccos - Google Patents
Extraction and purification method and detection method of arsenic form in paper for tobaccos Download PDFInfo
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- CN104451199A CN104451199A CN201410766666.8A CN201410766666A CN104451199A CN 104451199 A CN104451199 A CN 104451199A CN 201410766666 A CN201410766666 A CN 201410766666A CN 104451199 A CN104451199 A CN 104451199A
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Abstract
The invention belongs to the field of detection and relates to an extraction and purification method and a detection method of an arsenic form in paper for tobaccos. Particularly, the extraction and purification method comprises a step of adding an acid solution and an alcohol-ketone mixed liquid to a sample. The invention also relates to a combined reagent and an application of the combined reagent in extraction and purification or detection of the arsenic form in the paper for tobaccos. According to the extraction and purification method and the detection method disclosed by the invention, the blank for analyzing the arsenic form in the paper for tobaccos is filled; and the toxicity of arsenic in a paper material can be accurately and objectively controlled.
Description
Technical field
The invention belongs to material detection technique field, relate to one and to grow tobacco the extraction and purification methods of arsenic morphology in paper using and detection method.The invention still further relates to a kind of composite reagent and the extraction and cleaning of arsenic morphology or the purposes in detecting in tobacco paper using.
Background technology
Tobacco paper using comprises cigarette tissue, filter tip stick coil paper and cigarette tipping paper three kinds.Wherein, cigarette tissue is commonly called as obbbin, for rolling up pipe tobacco and participating in cigarette burning; Filter tip stick coil paper is wrapped in outside cigarette filter, plays and supports the shaping effect of filter tip; Cigarette tipping paper has another name called cork paper, is to be specifically designed to a kind of extra package paper using that filter tip is connected with cigarette, and cigarette tipping paper surface is generally brushed with brown or white coating, or ornamental in order to improve, and prints each colored pattern or trade mark title on paper.
Tobacco paper using is starting material indispensable during cigarette manufactures, the flue gas participating in burning generation due to cigarette tissue can affect environment, filter tip stick coil paper and cigarette tipping paper directly and oral contact can affect HUMAN HEALTH, therefore every country has strict requirement for the quality control of tobacco paper using, this is comprising arsenic, because arsenic is to the cardiac muscle of human body, respiratory system, neural system, reproductive system, hematopoiesis and immunity system all have damage in various degree, even with bring out lung cancer there is significant dependency, therefore the key concerning health of smokers is become to the control of arsenic content in tobacco paper using.
Along with the progress of science, investigator finds that the toxic action of arsenic is not only relevant with its content, also relevant with the form of arsenic.Arsenic morphology generally comprises arsenus acid (As (III)), arsenic acid (As (V)), monomethyl arsenic acid (MMA), dimethyl arsenate (DMA), arsenic trimethyl-glycine and arsenocholine, and arsenic sugar, arsenic ester compound etc.Find that the toxicity sequence of various arsenic morphology is arsenus acid > arsenic acid > monomethyl arsenic acid > dimethyl arsenate after deliberation, and arsenocholine and arsenic trimethyl-glycine nontoxic, the Difference In Toxicity of visible various arsenic morphology is comparatively large, only measure arsenic content in tobacco paper using cannot to the toxicity profile of arsenic in paper stock carry out objective, accurately control.Therefore, need badly and detection analysis is carried out to arsenic morphology, but there is no the method for tobacco paper using being carried out to arsenium morphological analysis at present.
Summary of the invention
Inventor, through deep research, obtains an extraction and purification methods growing tobacco arsenic morphology in paper using, and and then obtains the detection method of arsenic morphology in tobacco paper using.Method of the present invention can obtain the arsenic toxicity profile in tobacco paper using accurately, objectively.Thus provide following invention:
One aspect of the present invention provides an extraction and purification methods growing tobacco arsenic morphology in paper using, comprises the step adding acid solution and alcohol-one mixed solution in sample.Wherein, acid solution and alcohol-one mixed solution are simultaneously or asynchronously add; Particularly, in sample, first add acid solution, then add alcohol-one mixed solution.
In one embodiment of the invention, the amount of acid solution and alcohol-one mixed solution all can infiltrate sample; Particularly, acid solution is identical with the volume of alcohol-one mixed solution.
According to the extraction and purification methods of any one of the present invention, wherein, described acid solution is one or more in aqueous hydrochloric acid, aqueous sulfuric acid and aqueous acetic acid, and described acid solution can avoid the oxidation to low price arsenic morphology, and the reduction to high price arsenic morphology; Particularly, the sulfuric acid concentration of aqueous sulfuric acid is no more than 10% (w/w); Particularly, the pH value of aqueous hydrochloric acid is 5-6; Particularly, the aqueous hydrochloric acid of 10-15mL is added in every 2-4g sample.
According to the extraction and purification methods of any one of the present invention, wherein, described alcohol-one mixed solution is ethanol-acetone mixed solution or methanol-acetone mixed solution; Particularly, in ethanol-acetone mixed solution, the volume ratio of ethanol, acetone is 1:1.
According to the extraction and purification methods of any one of the present invention, wherein, under vortex oscillation, add acid solution and alcohol-one mixed solution; Particularly, the speed of vortex oscillation is 1500-2500r/min; Particularly, the time of vortex oscillation is 5-15min, is preferably 5-10min.
According to the extraction and purification methods of any one of the present invention, before it is also included in and adds acid solution and alcohol-one mixed solution, sample is carried out broken step; Particularly, be broken for described in and shred with ceramic scissors; Particularly, the sample area <3.5mm after shredding
2; Preferably, the sample area after shredding is 1-3mm
2, be more preferably 1mm
2, 2mm
2, 3mm
2.
On this basis, the present invention gives on the other hand a detection method growing tobacco arsenic morphology in paper using, comprises the extraction and purification methods of arsenic morphology in above-mentioned tobacco paper using; Particularly, also comprise the steps:
The liquid obtained by extraction and cleaning leaves standstill, filtration, then uses the content of different arsenic morphology in High performance liquid chromatography-inductively coupled plasma mass spectrometry combined instrument tracer liquid; Particularly, membrane filtration is filtered into described in; Preferably, the aperture of filter membrane is 0.22 μm.The liquid that the liquid that described extraction and cleaning obtains obtains after pointing to and adding acid solution and alcohol-one mixed solution extraction and cleaning in sample.
Aforesaid method is applicable to carry out extraction and cleaning or detection to the arsenic morphology in the tobacco paper usings such as cigarette tissue, filter tip stick coil paper or cigarette tipping paper.
The invention still further relates to a kind of composite reagent, comprise acid solution and alcohol-one mixed solution; Particularly, described composite reagent comprises aqueous hydrochloric acid and ethanol-acetone mixed solution; More specifically, the volume ratio of aqueous hydrochloric acid and ethanol-acetone mixed solution is 1:1; Particularly, in ethanol-acetone mixed solution, the volume ratio of ethanol, acetone is 1:1.
The invention still further relates to the extraction of described composite reagent arsenic morphology in tobacco paper using particularly cigarette tipping paper, purification or the purposes in detecting.
In the present invention, if not otherwise specified, term " arsenic morphology " refers to arsenic element in the environment with the physics of ion, molecule or other combination existence or chemical species.The arsenic morphology that the present invention extracts, purify or detect refers to trivalent arsenic (arsenus acid), pentavalent arsenic (arsenic acid), monomethyl arsenic acid (MMA) and/or dimethyl arsenate (DMA).
The beneficial effect of the invention
(1) the present invention has filled up the technological gap of arsenic morphology extraction and cleaning, detection method in existing tobacco paper using, can reflect the fractions distribution situation of arsenic in paper stock accurately, objectively, for production low toxicity, nontoxic tobacco paper using provide guarantee.
(2) the present invention adopt acid solution and polar-nonpolar organic liquid mixture combined, ensure that in paper stock, various arsenic morphology is separated and is uniformly distributed in a liquid, thus facilitate disposable sampling to detect.
(3) extraction and cleaning of the present invention is simple, relative deviation is little, the rate of recovery is high.
Accompanying drawing explanation
Fig. 1: the schema of arsenic morphology detection method in tobacco paper using of the present invention.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturers suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
In cigarette tipping paper, the detection method of arsenic morphology as shown in Figure 1.
embodiment 1:
Take about 2g cigarette tipping paper (production of Hengfeng paper mill, Zhejiang), be cut into about 1mm with ceramic scissors
2sample be put in 50mL tool lid centrifuge tube, add 10mL, pH value is the aqueous hydrochloric acid of 5, the velocity fluctuation 5min be placed in 1500r/min on whirlpool mixing shaker makes sample fully infiltrate, add the ethanol-acetone mixed solution of 10mL, volume ratio 1:1 again, continue with 1500r/min velocity fluctuation 10min on whirlpool mixing shaker, getting supernatant liquor via hole diameter after leaving standstill is sample introduction after the membrane filtration of 0.22 μm.Adopt High performance liquid chromatography-inductively coupled plasma mass spectrometry combined instrument (U.S. Aglient1260 high performance liquid chromatography and the coupling of U.S. Aglient7500 inductivity coupled plasma mass spectrometry) to detect, result is as shown in table 1.
Take many parts and be cut into about 1mm
2above-mentioned cigarette tipping paper sample (being 3g), put into multiple centrifuge tube respectively.Added respectively in different centrifuge tube by the pentavalent arsenic standardized solution of the monomethyl arsenic standard solution of the trivalent arsenic standardized solution of 0.5mg/L, 2mg/L, the dimethyl arsenic standard solution of 5mg/L and 0.5mg/L, add-on is 0.05mL; Then all add 10mL, pH value be 5 aqueous hydrochloric acid infiltrate, impregnation process and subsequent operations same as described above, each standardized solution repeats three samples and averages, and calculates the rate of recovery and relative standard deviation according to the following formula, the results are shown in Table 1.
The rate of recovery=(mark-on sample measurements-sample measurements)/add scalar × 100%
Wherein, mark-on sample measurements is the assay value after adding different shape arsenic standard solution in sample, and adding scalar is arsenic total amount in the arsenic standard solution added.
Table 1
Found that, detect the rate of recovery of various arsenic morphology in sample all between 80 ~ 120%, relative deviation R.S.D is less than 5%, meets Physico-chemical tests requirement, can reflect the fractions distribution situation of arsenic in paper stock accurately, objectively.
embodiment 2:
Take about 4g cork paper (a kind of cigarette tipping paper, by the people live in plenty in Zhejiang paper mill produces) to shred into about 3mm with ceramic scissors
2sample in 50mL tool lid centrifuge tube, add 15mL, pH value is the aqueous hydrochloric acid of 6, the velocity fluctuation 10min be placed in 2500r/min on whirlpool mixing shaker makes sample fully infiltrate, add the methanol-acetone mixed solution of 15mL, volume ratio 1:1 again, continue with 2500r/min velocity fluctuation 15min on whirlpool mixing shaker, getting supernatant liquor via hole diameter after leaving standstill is sample introduction after the membrane filtration of 0.22 μm.Adopt the High performance liquid chromatography-inductively coupled plasma mass spectrometry combined instrument in embodiment 1 to detect, result is as shown in table 2.
Take many parts and be cut into about 3mm
2above-mentioned sample (being 3g), put into multiple centrifuge tube respectively.Added respectively in different centrifuge tube by the pentavalent arsenic standardized solution of the monomethyl arsenic standard solution of the trivalent arsenic standardized solution of 0.5mg/L, 2mg/L, the dimethyl arsenic standard solution of 5mg/L and 0.5mg/L, add-on is 0.05mL; Then all add 10mL, pH value be 5 aqueous hydrochloric acid infiltrate, impregnation process and subsequent operations same as described above, each standardized solution repeats three samples and averages, and calculates the rate of recovery and relative standard deviation, the results are shown in Table 2 according to embodiment 1 method.
Table 2
Found that, detect the rate of recovery of various arsenic morphology in sample all between 80 ~ 120%, relative deviation R.S.D is less than 5%, meets Physico-chemical tests requirement, can reflect the fractions distribution situation of arsenic in paper stock accurately, objectively.
embodiment 3:
Take about 3g cigarette tissue (Zhejiang the people live in plenty paper mill) to shred into about 2mm with ceramic scissors
2sample in 50mL tool lid centrifuge tube, add 12.5mL, aqueous sulfuric acid that content is 8% (w/w), the velocity fluctuation 7.5min be placed in 2000r/min on whirlpool mixing shaker makes sample fully infiltrate, add the ethanol-acetone mixed solution of 12.5mL, volume ratio 1:1 again, continue with the velocity fluctuation 12.5min of 2000r/min on whirlpool mixing shaker, getting supernatant liquor via hole diameter after leaving standstill is sample introduction after the membrane filtration of 0.22 μm.Adopt the High performance liquid chromatography-inductively coupled plasma mass spectrometry combined instrument in embodiment 1 to detect, result is as shown in table 3.
Take many parts and be cut into about 2mm
2above-mentioned sample (being 3g), put into multiple centrifuge tube respectively.Added respectively in different centrifuge tube by the pentavalent arsenic standardized solution of the monomethyl arsenic standard solution of the trivalent arsenic standardized solution of 0.5mg/L, 2mg/L, the dimethyl arsenic standard solution of 5mg/L and 0.5mg/L, add-on is 0.05mL; Then all add 10mL, pH value be 5 aqueous hydrochloric acid infiltrate, impregnation process and subsequent operations same as described above, each standardized solution repeats three samples and averages, and calculates the rate of recovery and relative standard deviation, the results are shown in Table 3 according to embodiment 1 method.
Table 3
Found that, detect the rate of recovery of various arsenic morphology in sample all between 80 ~ 120%, relative deviation R.S.D is less than 5%, meets Physico-chemical tests requirement, can reflect the fractions distribution situation of arsenic in paper stock accurately, objectively.
Except the cigarette tipping paper of above-described embodiment, method of the present invention is also applicable to extraction and cleaning and the detection of the tobacco paper usings such as cigarette tissue, filter tip stick coil paper being carried out to arsenic morphology.
Although the specific embodiment of the present invention has obtained detailed description, it will be understood to those of skill in the art that.According to disclosed all instructions, can carry out various amendment and replacement to those details, these change all within protection scope of the present invention.Four corner of the present invention is provided by claims and any equivalent thereof.
Claims (10)
1. an extraction and purification methods growing tobacco arsenic morphology in paper using, comprises the step adding acid solution and alcohol-one mixed solution in sample.
2. extraction and purification methods according to claim 1, wherein, described acid solution and alcohol-one mixed solution are simultaneously or asynchronously add; Particularly, in sample, first add acid solution, then add alcohol-one mixed solution.
3. extraction and purification methods according to claim 2, wherein, the amount of described acid solution and alcohol-one mixed solution all can infiltrate sample; Particularly, acid solution is identical with the volume of alcohol-one mixed solution.
4. according to the arbitrary described extraction and purification methods of claim 1-3, wherein, described acid solution is one or more in aqueous hydrochloric acid, aqueous sulfuric acid and aqueous acetic acid; Particularly, the sulfuric acid concentration of aqueous sulfuric acid is no more than 10% (w/w); Particularly, the pH value of aqueous hydrochloric acid is 5-6; More specifically, the aqueous hydrochloric acid of 10-15mL is added in every 2-4g sample.
5., according to the arbitrary described extraction and purification methods of claim 1-4, wherein, described alcohol-one mixed solution is ethanol-acetone mixed solution or methanol-acetone mixed solution; Particularly, in ethanol-acetone mixed solution, the volume ratio of ethanol, acetone is 1:1.
6. extraction and purification methods according to claim 1, wherein, adds acid solution and alcohol-one mixed solution under vortex oscillation; Particularly, the speed of vortex oscillation is 1500-2500r/min; Particularly, the time of vortex oscillation is 5-15min, is preferably 5-10min.
7. extraction and purification methods according to claim 1, before it is also included in and adds acid solution and alcohol-one mixed solution, carries out broken step by sample; Particularly, be broken for described in and shred with ceramic scissors; Particularly, the sample area <3.5mm after shredding
2; Preferably, the sample area after shredding is 1-3mm
2.
8. a detection method growing tobacco arsenic morphology in paper using, comprises the extraction and purification methods of arsenic morphology in the arbitrary described tobacco paper using of claim 1-7; Particularly, also comprise the steps:
The liquid obtained by extraction and cleaning leaves standstill, filtration, then uses the content of different arsenic morphology in High performance liquid chromatography-inductively coupled plasma mass spectrometry combined instrument tracer liquid; Particularly, membrane filtration is filtered into described in; Preferably, the aperture of filter membrane is 0.22 μm.
9. a composite reagent, comprises acid solution and alcohol-one mixed solution; Particularly, described composite reagent comprises aqueous hydrochloric acid and ethanol-acetone mixed solution; More specifically, the volume ratio of aqueous hydrochloric acid and ethanol-acetone mixed solution is 1:1; Particularly, in ethanol-acetone mixed solution, the volume ratio of ethanol, acetone is 1:1.
10. the extraction of the arsenic morphology in tobacco paper using particularly cigarette tipping paper of composite reagent described in claim 9, purification or the purposes in detecting.
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