CN101393180B - Method for measuring beta-naphthol content in additive agent for cigarette - Google Patents
Method for measuring beta-naphthol content in additive agent for cigarette Download PDFInfo
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- CN101393180B CN101393180B CN2008102306571A CN200810230657A CN101393180B CN 101393180 B CN101393180 B CN 101393180B CN 2008102306571 A CN2008102306571 A CN 2008102306571A CN 200810230657 A CN200810230657 A CN 200810230657A CN 101393180 B CN101393180 B CN 101393180B
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Abstract
The invention relates to a method for mensurating the content of beta-naphthol in a cigarette additive. The method is characterized by comprising the following steps: a. a sample is weighed and is put to a vessel; b. a naphthalene-containing methylene dichloride solution as an extracting solution is added into the sample; c. anhydrous sodium sulfate is added into a mixture; d. the mixture is oscillated and extracted; a supernatant fluid is taken out and is used as a sample extracting solution; e. a standard working solution is prepared; a beta-naphthol standard sample is weighed; the naphthalene-containing methylene dichloride solution is dissolved and has constant volume; further, the naphthalene-containing methylene dichloride solution is diluted to be standard working solution with concentration grads; and f. the prepared beta-naphthol standard working solutions with different concentration is injected to GC/MS; and the content of beta-naphthol is subjected to quantitative analysis by an internal standard method. The method adopts a gas chromatography-mass spectrometer (GC/MS) to directly mensurate the content of the beta-naphthol in cigarette essence and spice, and has the advantages of simple, rapid and accurate operation, high sensitivity and good repeatability.
Description
Technical field:
The invention belongs to the physical and chemical inspection technical field of cigarette additive, relate generally to the assay method of beta-naphthol content in the cigarette additive, is to adopt gas chromatograph-mass spectrometer (GCMS) (GC/MS) directly to measure the method for beta-naphthol content in the cigarette additive specifically.
Background technology:
In cigarette product design and process of manufacture, for improving product quality and satisfying process requirements, enterprise often needs choosing to add such as adjuvants such as sweetener, antiseptic, humectant, combustion adjuvant, plastifier.The use of these adjuvants is one of important factor in order of cigarette product quality and security.
Betanaphthol claims beta naphthal again, is the raw material of producing medicine, dyestuff, spices, synthetic rubber antioxidant etc., also can be used as expelling parasite, germifuge and antiseptic.Betanaphthol belongs to medium malicious class material, and eyes, skin, mucous membrane are had the intense stimulus effect; To the kidney nephritis that can cause bleeding; After wrongly taking, vomiting, diarrhoea, stomachache, spasm, anaemia, collapse can appear; Betanaphthol contacts with local skin can cause decortication, even produces permanent pigmentation.
Betanaphthol is that cigarette bans use of adjuvant.Because the laws and regulations on the management of China's tobacco additive agent are perfect not enough, betanaphthol might enter cigarette product in the reinforced process of perfuming cigarette but at present.Do not see at present the detection method bibliographical information of betanaphthol in the essence spice for cigarette.
Detection method bibliographical information about betanaphthol in other material has: the quality inspection that GB/T1646-2003 " GB/T1646-20032-naphthols " has stipulated the reversed-phase HPLC-UV of beta naphthal, be mainly used in industry such as dyestuff, rubber and paint, also can be used for medicine and spices, the analysis foundation that provides for the quality monitoring of this series products, but HPLC-UV sensitivity is lower, selects quantitative precision relatively poor to complex sample; Zhou Hua etc. " Zhou Hua, Zhang Guoqi, Gao Yan, Liu Hongying, Long Feng; chemical substance in the gas chromatography determination oxidative hair dyes; Chinese public health, 2003,19 (08): 996. " extract sample with the ethanol sonic oscillation after, constant volume, get in the supernatant inject gas chromatograph with microsyringe, measured the content of betanaphthol in the oxidative hair dyes, but this method detects with GC-FID, sensitivity is low, and complex sample is still needed adopt GC/MS to prove conclusively.
Summary of the invention:
Purpose of the present invention is intended to overcome the prior art defective, provide a kind of employing gas chromatograph-mass spectrometer (GCMS) (GC/MS) directly to measure the method for beta-naphthol content in the cigarette additive, this method can fast, accurately detect beta-naphthol content in the cigarette additive, and measurement result is accurate, mensuration is disturbed few.
The objective of the invention is to be achieved through the following technical solutions: the assay method of beta-naphthol content may further comprise the steps in the cigarette additive of the present invention:
A, take by weighing sample, put into container;
B, add extract, for containing the dichloromethane solution of naphthalene;
C, adding anhydrous sodium sulfate;
D, vibration are extracted, and get supernatant and are sample extracting solution;
E, preparation standard operation solution.Take by weighing the betanaphthol standard items, with the methylene chloride dissolving and the constant volume that contain naphthalene, then further with the standard operation solution of methylene chloride dilution that contains naphthalene for having concentration gradient;
F, the betanaphthol standard operation solution of the variable concentrations for preparing is injected GC/MS, carry out the quantitative test of beta-naphthol content with internal standard method, promptly compare its respective concentration and carry out regretional analysis with the chromatographic peak area of betanaphthol and interior mark naphthalene, obtain typical curve, related coefficient is measured the sample after extracting more than or equal to 0.999, records the chromatographic peak area ratio of betanaphthol and interior mark naphthalene, the substitution typical curve is tried to achieve the beta-naphthol content in the sample.
Used GC/MS analysis condition is in step f of the present invention: chromatographic column: HP-VOC fused quartz capillary column (60m * 0.32mm i.d. * 1.8 μ m d.f.); Injector temperature: 230 ℃, sample size: 2 μ L; Carrier gas: He, split ratio 5:1, flow velocity 2.5mL/min; Temperature programme:
Transmission line temperature: 280 ℃; Ionization (E1) energy: 70eV; Ion source temperature: 230 ℃; Solvent delay 8min selects ion mode (SIM) scanning, and the selection ion of betanaphthol is 144,115, and the selection ion of naphthalene is 128,102.
Above-mentioned standard operation solution with concentration gradient, its concrete compound method is as follows: take by weighing the 0.0200g betanaphthol, with the dissolving of the dichloromethane solution of naphthalene and be settled to 100mL, be mixed with the betanaphthol mother liquor of 200 μ g/mL, the betanaphthol mother liquor that accurately pipettes different volumes is to the 10mL volumetric flask, dichloromethane solution constant volume with naphthalene, be mixed with the betanaphthol standard operation solution of variable concentrations, standard sequence: 0.001 μ g/mL, 0.004 μ g/mL, 0.016 μ g/mL, 0.08 μ g/mL, 0.40 μ g/mL, 2.0 μ g/mL, 10.0 μ g/mL.Calculate by taking by weighing the 0.2g additive samples, promptly obtain standard sequence: 0.05 μ g/g, 0.20 μ g/g, 0.80 μ g/g, 4.00 μ g/g, 20.00 μ g/g, 100.00 μ g/g, 500.00 μ g/g.
In the present invention, the concentration of naphthalene is 0.77 μ g/mL in the dichloromethane solution of employed naphthalene.Anhydrous sodium sulfate with preceding in muffle furnace 550 ℃ of following baking 4h.
Method of the present invention has overcome the deficiency of prior art sample treatment, has optimized sample-pretreating method and instrument detecting condition at the essence spice for cigarette sample.Compared with prior art the inventive method has following excellent results:
(1) the essence spice for cigarette sample is soluble perfume mostly, solvent commonly used has water, ethanol, propylene glycol and glycerine, moisture in the sample damages bigger to capillary chromatographic column and GC/MS detection system, historical facts or anecdotes test selection with anhydrous sodium sulfate as drying agent, remove the moisture in the sample.
(2) for the mensuration of betanaphthol, prior art is many with the external standard standard measure, but for the bigger essence spice for cigarette sample of viscosity, with the external standard standard measure, constant volume gets up cumbersome.And utilize inner mark method ration, by the adding of internal standard compound, utilize the relative peak area value of component to carry out the calculating of some quantized datas, can be without constant volume, and can reduce the error of being brought by pre-treating method reappearance and instrument precision problem, so this law adopts inner mark method ration.The flavor component that tolerable adds in the essence spice for cigarette is more, so its complicated component is difficult to select a suitable internal standard compound as object of reference, naphthalene has the coal tar stink, can not be added in the essence and flavoring agent, so the present invention selects naphthalene as interior mark.
(3) the inventive method has selected the best HP-VOC post of peak shape and separating effect as separating column, and adopts the GC/MS that can provide qualitative and quantitative information simultaneously as detection mode, has guaranteed the accuracy of testing result.
(4) this method has the advantage of easy and simple to handle, quick, accurate, highly sensitive and good reproducibility.
1. the detectability of the inventive method
The betanaphthol standard operation solution of variable concentrations is injected GC/MS, calculate detectability with 3 times of signal to noise ratio (S/N ratio)s (S/N=3), the result is 0.01 μ g/g.
2. repeatability of the inventive method and recovery of standard addition
The standard solution that adds betanaphthol in not containing the essence spice for cigarette sample of betanaphthol carries out pre-treatment and GC/MS then respectively and analyzes, and calculates its recovery according to adding the scalar sum measured value, the results are shown in Table 1.As can be seen from Table 1, on 3 mark-on levels, the average recovery rate of betanaphthol is 96.55%, and average relative standard deviation (RSD) is 2.35%, illustrates that the recovery of the inventive method is higher, good reproducibility.
The recovery of table 1 betanaphthol and repeatability (n=6)
Description of drawings
Accompanying drawing is assay method process flow diagram of the present invention (this figure is as Figure of abstract).
Embodiment
The present invention is described further below in conjunction with example, but is not restriction the present invention.
Example 1:
1. instrument and reagent:
Betanaphthol is analyzed pure; Naphthalene is analyzed pure; Anhydrous Na
2SO
4, analyze pure; Methylene chloride, chromatographic grade; Analytical balance, sensibility reciprocal: 0.0001g; Horizontal cyclotron oscillation device; Gas chromatograph-mass spectrometer (GCMS) (GC/MS).
2. sample preparation:
Anhydrous sodium sulfate: with preceding in muffle furnace 550 ℃ the baking 4h.
Get essence sample 0.20g, accurately add the dichloromethane solution (concentration of naphthalene is 0.77 μ g/mL) of 10mL naphthalene, add the 5g anhydrous sodium sulfate then, vibration 30min leaves standstill 10min, gets supernatant and carries out the GC/MS analysis.
3. standard solution configuration
Take by weighing the 0.0200g betanaphthol, with the dissolving of the dichloromethane solution of naphthalene and be settled to 100mL, be mixed with the betanaphthol mother liquor of 200 μ g/mL, the betanaphthol mother liquor that accurately pipettes different volumes is to the 10mL volumetric flask, with the dichloromethane solution constant volume of naphthalene, be mixed with the betanaphthol standard operation solution of variable concentrations, standard sequence: 0.001 μ g/mL, 0.004 μ g/mL, 0.016 μ g/mL, 0.08 μ g/mL, 0.40 μ g/mL, 2.0 μ g/mL, 10.0 μ g/mL.Calculate by taking by weighing 0.2g essence and flavoring agent sample, promptly obtain standard sequence: 0.05 μ g/g, 0.20 μ g/g, 0.80 μ g/g, 4.00 μ g/g, 20.00 μ g/g, 100.00 μ g/g, 500.00 μ g/g.
4. assay method:
The betanaphthol standard operation solution of the variable concentrations for preparing is injected GC/MS, compare its respective concentration with the chromatographic peak area of betanaphthol and interior mark naphthalene and carry out regretional analysis, obtain typical curve.Sample after extracting is measured, recorded the chromatographic peak area ratio of betanaphthol and interior mark naphthalene, the substitution typical curve, the beta-naphthol content of trying to achieve in the sample is 1.32 μ g/g.
The GC/MS analysis condition is: chromatographic column: HP-VOC fused quartz capillary column (60m * 0.32mmi.d. * 1.8 μ m d.f.); Injector temperature: 230 ℃, sample size: 2 μ L; Carrier gas: He, split ratio 5:1, flow velocity 2.5mL/min; Temperature programme:
Transmission line temperature: 280 ℃; Ionization (E1) energy: 70eV; Ion source temperature: 230 ℃; Solvent delay 8min selects ion mode (SIM) scanning, and the selection ion of betanaphthol is 144,115, and the selection ion of naphthalene is 128,102.
Accuracy for determination methods, the betanaphthol standard solution that in this essence sample, adds 1.16 μ g/g, carry out the same sample pre-treatments, record the chromatographic peak area ratio of betanaphthol and interior mark naphthalene with GC/MS, the substitution typical curve, the beta-naphthol content of trying to achieve in sample this moment is 2.45 μ g/g, and promptly the recovery of standard addition of sample 4.00 μ g/g is 97.41%, illustrates that the method is accurately.
Claims (3)
1. the assay method of beta-naphthol content in the cigarette additive is characterized in that: may further comprise the steps:
A, take by weighing sample, put into container;
B, add extract, for containing the dichloromethane solution of naphthalene, the concentration of naphthalene is 0.77 μ g/mL in the dichloromethane solution of naphthalene;
C, adding anhydrous sodium sulfate;
D, vibration are extracted, and get supernatant and are sample extracting solution;
E, preparation standard operation solution take by weighing the betanaphthol standard items, use the methylene chloride dissolving and the constant volume that contain naphthalene, and further diluting with the methylene chloride that contains naphthalene then is the standard operation solution with concentration gradient;
F, the betanaphthol standard operation solution of the variable concentrations for preparing is injected GC/MS, carry out the quantitative test of beta-naphthol content with internal standard method, promptly compare its respective concentration and carry out regretional analysis with the chromatographic peak area of betanaphthol and interior mark naphthalene, obtain typical curve, related coefficient is measured the sample after extracting more than or equal to 0.999, records the chromatographic peak area ratio of betanaphthol and interior mark naphthalene, the substitution typical curve is tried to achieve the beta-naphthol content in the sample;
The GC/MS analysis condition is: chromatographic column: HP-VOC fused quartz capillary column 60m * 0.32mm i.d. * 1.8 μ m d.f.; Injector temperature: 230 ℃, sample size: 2 μ L; Carrier gas: He, split ratio 5: 1, flow velocity 2.5mL/min; Temperature programme: 40 ℃ keep 1min, are warming up to 245 ℃ with 20 ℃/min and keep 10min; Transmission line temperature: 280 ℃; Ionization EI energy: 70eV; Ion source temperature: 230 ℃; Solvent delay 8min selects ion mode scanning, and the selection ion of betanaphthol is 144,115, and the selection ion of naphthalene is 128,102.
2. the assay method of beta-naphthol content in the cigarette additive according to claim 1, it is characterized in that: the concrete compound method with concentration gradient standard operation solution is: take by weighing the 0.0200g betanaphthol, with the dissolving of the dichloromethane solution of naphthalene and be settled to 100mL, be mixed with the betanaphthol mother liquor of 200 μ g/mL, the betanaphthol mother liquor that accurately pipettes different volumes is to the 10mL volumetric flask, dichloromethane solution constant volume with naphthalene, be mixed with the betanaphthol standard operation solution of variable concentrations, standard sequence: 0.001 μ g/mL, 0.004 μ g/mL, 0.016 μ g/mL, 0.08 μ g/mL, 0.40 μ g/mL, 2.0 μ g/mL, 10.0 μ g/mL; Calculate by taking by weighing the 0.2g additive samples, promptly obtain standard sequence: 0.05 μ g/g, 0.20 μ g/g, 0.80 μ g/g, 4.00 μ g/g, 20.00 μ g/g, 100.00 μ g/g, 500.00 μ g/g.
3. the assay method of beta-naphthol content in the cigarette additive according to claim 1 is characterized in that: anhydrous sodium sulfate with preceding in muffle furnace 550 ℃ of following baking 4h.
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| CN101819192A (en) * | 2010-05-14 | 2010-09-01 | 唐山建龙实业有限公司 | Method for detecting naphthalene content in washing oil by gas chromatography |
| CN102072940B (en) * | 2010-11-11 | 2012-11-28 | 中国烟草总公司湖北省公司 | Method for measuring contents of coumarin and safrole in flavor and fragrance for cigarette |
| CN102253147B (en) * | 2011-07-19 | 2014-04-09 | 中国烟草总公司郑州烟草研究院 | Method for measuring content of dihydrocoumarin and 6-methyl coumarin in additive for tobaccos |
| CN102608244A (en) * | 2012-03-02 | 2012-07-25 | 红云红河烟草(集团)有限责任公司 | Detection method for simultaneously determining plurality of flavor substances in cigarette cut tobaccos |
| CN103115971B (en) * | 2012-11-27 | 2014-08-20 | 广西中烟工业有限责任公司 | Detection method of synthetic phenol antioxidants in flavors and fragrances for cigarettes |
| CN103698455B (en) * | 2013-12-20 | 2015-06-03 | 南京工业大学 | Analysis method of reaction liquor and product in synthesis of naphthol by virtue of catalytic oxidation of naphthalene |
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