CN110806391A - Method for detecting oil stain on surface of dropping pill for cigarettes - Google Patents
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- CN110806391A CN110806391A CN201911087431.5A CN201911087431A CN110806391A CN 110806391 A CN110806391 A CN 110806391A CN 201911087431 A CN201911087431 A CN 201911087431A CN 110806391 A CN110806391 A CN 110806391A
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- 239000006187 pill Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 27
- 238000010521 absorption reaction Methods 0.000 claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 15
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims abstract description 11
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 62
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 21
- 238000002835 absorbance Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000012088 reference solution Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000012417 linear regression Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 3
- 238000002211 ultraviolet spectrum Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides a method for detecting the oil stain on the surface of a dropping pill for cigarettes, which comprises the following steps: preparing a test sample, determining the optimal ultraviolet absorption wavelength, drawing a standard curve, and detecting the oil stain content. The invention adopts an ultraviolet-visible spectrophotometry to establish a method for detecting the oil stain on the surface of the dropping pill for cigarettes, has simple operation, and can quickly and accurately determine the white oil content on the surface of the dropping pill; in addition, the anhydrous sodium sulfite is used in the process of preparing the test sample to eliminate the measurement error caused by oxidation of white oil in the detection process, so that the detection result is more accurate and reliable. The method is mainly suitable for measuring the oil stain on the surface of the wet pills, and the detection limit of white oil on the surface of the dripping pills is 0.05 mg/g-0.4 mg/g.
Description
Technical Field
The invention relates to the technical field of tobacco,
in particular to a method for detecting the oil stain on the surface of a dropping pill for cigarettes.
Background
In recent years, the dropping pill cigarette for cigarettes endows consumers with fresh and comprehensive experience to cigarette products from sensory dimensions such as smell, touch, hearing and the like. The perfuming of the dropping pills for cigarettes is a new bright point for increasing the pulling quantity and improving the structure by taking the specific advantages thereof as the trend of accelerating development in the industry, and compared with other flavoring technologies, the dropping pills for cigarettes can realize artificial controllable fragrance release in the process of smoking cigarettes, enrich the smoking taste of the cigarettes, and endow the cigarettes with characteristic fragrance or improve the comfort of the cigarettes. The production process flow of the dropping pill for the cigarette comprises the following steps: online forming, deoiling, drying, screening and balancing. On-line forming of the drop pills needs to be done in a cooling oil system, resulting in a large amount of oily solvent adhering to the surface of the wet pills. After dripping and forming, the wet pills need to be deoiled, and if the deoiling effect is not ideal, oil stains can be formed on the surfaces of the dripping pills, so that the product quality is influenced.
The main component of the oil stain on the surface of the dripping pill is white oil by combining the analysis of the production process condition. The traditional method for measuring the components of the oil mainly measures the saponification value, the iodine value and the acid value of the oil, and can obtain the content of total unsaturated fatty acid in the oil. If the type and the content of unsaturated fatty acid are to be determined, gas chromatography and high performance liquid chromatography are generally adopted at present, and both a sample to be detected needs to be pretreated, so that the steps are long and complicated, and the detection is long.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for detecting the oil stain on the surface of a dropping pill for cigarettes.
In order to solve the problems, the invention adopts the following technical scheme:
a method for detecting oil stain on the surface of a dropping pill for cigarettes comprises the following steps:
preparation of test samples: extracting the dropping pill to be detected by using normal hexane and anhydrous sodium sulfite to obtain a mixed solution containing oil stains;
determining the optimal ultraviolet absorption wavelength: preparing white oil into a solution with the mass fraction of 1% by using n-hexane, taking analytically pure n-hexane as a blank, carrying out wavelength scanning on an ultraviolet-visible spectrophotometer, wherein the scanning wavelength range is 190-400 nm, the scanning speed is medium, the sampling interval is 0.2nm, the slit width is 1.0nm, the thickness of a quartz cuvette is 1cm, and analyzing the absorption peak of an ultraviolet spectrum after scanning for 3 times to determine the optimal absorption wavelength;
drawing a standard curve: preparing a series of standard white oil samples with different concentrations by using n-hexane, sequentially measuring the absorbance values of the samples at the optimal ultraviolet absorption wavelength on an ultraviolet-visible spectrophotometer according to the sequence of the concentration from low to high, and performing linear regression on the absorbance values and the white oil content to obtain a standard curve;
detecting the oil stain content: at the optimal ultraviolet absorption wavelength, putting n-hexane serving as a reference solution into a quartz cuvette, and adjusting zero; and testing the absorbance of the mixed solution, and calculating the surface oil stain quantity of the dropping pill to be tested by using the standard curve.
Preferably, the preparation of the test sample is performed as follows: putting 80-100 g of dropping pills to be tested into a beaker, adding 300mL of 95% hot ethanol, soaking for 10-15 min to remove surface white oil, filtering and draining by adopting a screen, weighing 10-50 g of ethanol solution containing the white oil, putting the ethanol solution into a separating funnel, adding 25mL of n-hexane and 5-10 g of anhydrous sodium sulfite, violently shaking and mixing for 1-3 min, standing until the solution is transparent, adding 25mL of n-hexane after separating, and extracting for 2-3 times to obtain the mixed solution containing oil stains.
Preferably, the optimal absorption wavelength is 277.10 nm.
Preferably, the detection limit of white oil on the surface of the dripping pill is 0.05 mg/g-0.4 mg/g.
Compared with the prior art, the invention has the technical effects that:
the invention adopts an ultraviolet-visible spectrophotometry to establish a method for detecting the oil stain on the surface of the dropping pill for cigarettes, has simple operation, and can quickly and accurately determine the white oil content on the surface of the dropping pill; in addition, the anhydrous sodium sulfite is used in the process of preparing the test sample to eliminate the measurement error caused by oxidation of white oil in the detection process, so that the detection result is more accurate and reliable. The method is mainly suitable for measuring the oil stain on the surface of the wet pills, and the detection limit of white oil on the surface of the dripping pills is 0.05 mg/g-0.4 mg/g.
Drawings
FIG. 1 is a standard curve of a standard white oil sample provided by an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for detecting oil stain on the surface of a dropping pill for cigarettes, which comprises the following steps:
(1) preparation of test samples: extracting the dropping pill to be detected by using normal hexane and anhydrous sodium sulfite to obtain a mixed solution containing oil stains;
(2) determining the optimal ultraviolet absorption wavelength: preparing white oil into a solution with the mass fraction of 1% by using n-hexane, taking analytically pure n-hexane as a blank, carrying out wavelength scanning on an ultraviolet-visible spectrophotometer UV-755B, wherein the scanning wavelength range is 190-400 nm, the scanning speed is medium, the sampling interval is 0.2nm, the slit width is 1.0nm, the thickness of a quartz cuvette is 1cm, analyzing an absorption peak of an ultraviolet spectrum after scanning for 3 times, and determining that the optimal absorption wavelength is 277.10 nm;
(3) drawing a standard curve: preparing a series of standard white oil samples with different concentrations by using n-hexane, sequentially measuring the absorbance values of the samples at the optimal ultraviolet absorption wavelength on an ultraviolet-visible spectrophotometer according to the sequence of the concentration from low to high, and performing linear regression on the absorbance values and the white oil content to obtain a standard curve;
specifically, 5g of white oil is weighed and added into a 50ml volumetric flask, and normal hexane is used for fixing the volume to a specified scale to prepare a white oil standard solution of 100 mg/ml. Precisely measuring 0.50ml, 1.00ml, 2.00ml, 3.0ml and 4.0ml of white oil standard solution respectively, and fixing the volume to a 50ml volumetric flask by using n-hexane to obtain white oil solutions with the concentrations of 1mg/ml, 2mg/ml, 4mg/ml, 6mg/ml and 8mg/ml respectively. The absorbance values of the five samples were sequentially measured in the order of concentration from low to high, and linear regression was performed using the absorbance value (y) as the abscissa and the white oil content (x, mg/m 1) as the ordinate to obtain a standard curve equation of y =0.095x +0.029 (R2=0.999), and the standard curve is shown in fig. 1.
(4) Detecting the oil stain content: at the optimum ultraviolet absorption wavelength of 277.10nm, putting n-hexane as a reference solution into a quartz cuvette, and adjusting zero; and adding 1ml of mixed solution into a quartz dish, starting reading, recording absorbance values, measuring the sample for 3 times, taking an average value, and calculating the surface oil stain amount of the dropping pill to be measured by using a standard curve.
Preferably, the step (1) of preparing the test sample is carried out by the following procedure: putting 80-100 g of dropping pills to be tested into a beaker, adding 300mL of 95% hot ethanol, soaking for 10-15 min to remove surface white oil, filtering and draining by adopting a screen, weighing 10-50 g of ethanol solution containing the white oil, placing the ethanol solution into a separating funnel, adding 25mL of n-hexane and 5-10 g of anhydrous sodium sulfite, violently shaking and mixing for 1-3 min, standing until the solution is transparent, adding 25mL of n-hexane after separating, and extracting for 2-3 times to obtain a mixed solution containing oil stains. The white oil has good solubility in 95% hot ethanol, and the white oil on the surface of the dripping pill is eluted by the hot ethanol to obtain an ethanol solution containing the white oil; in the subsequent operation process, along with the temperature reduction, the solubility of the white oil in the ethanol is gradually reduced, and the mixed solution of the white oil-containing n-hexane is obtained by matching with the extraction effect of the n-hexane and is used as a sample to be detected.
The detection method for the oil stain on the surface of the dropping pill for the cigarette has the detection limit of 0.05 mg/g-0.4 mg/g for white oil.
The invention adopts an ultraviolet-visible spectrophotometry to establish a method for detecting the oil stain on the surface of the dropping pill for cigarettes, has simple operation, and can quickly and accurately determine the white oil content on the surface of the dropping pill; in addition, the anhydrous sodium sulfite is used in the process of preparing the test sample to eliminate the measurement error caused by oxidation of white oil in the detection process, so that the detection result is more accurate and reliable.
The following is a further description with reference to specific examples.
Example 1
The embodiment 1 of the invention provides a method for detecting oil stain on the surface of a dropping pill for cigarettes, which comprises the following steps:
(1) preparation of test samples: randomly putting 100g of dropping pills to be tested from a dropping pill production line into a beaker, adding 300mL of 95% hot ethanol, soaking for 15min to remove white oil, filtering and draining by adopting a screen, weighing 30g of ethanol solution containing the white oil, putting the ethanol solution into a separating funnel, adding 25mL of n-hexane and 8g of anhydrous sodium sulfite, violently shaking and mixing for 3min, standing until the solution is transparent, adding 25mL of n-hexane after separating, extracting for 3 times to obtain a mixed solution containing oil stains, and fixing the volume to 50mL by using the n-hexane.
(2) And (3) detecting the absorbance of the test sample: starting an ultraviolet-spectrophotometer, preheating, setting the detection wavelength to 277.10nm, putting n-hexane as a reference solution into a quartz cuvette, and adjusting zero. 1ml of the mixed solution prepared in step (1) was taken and put into a quartz dish to start reading and record the absorbance value, and the average absorbance value of the sample measured 3 times was 0.374.
(3) Calculating the white oil content of the test sample: substituting the sample absorbance value of 0.374 into the standard curve equation y =0.095x +0.029 calculates the white oil content of the sample as: c = (0.374-0.029)/0.095 =3.63 (mg/ml), so the white oil concentration per gram of dropping pill is: c =3.63/30=0.121 (mg/ml).
Example 2
The embodiment 2 of the invention provides a method for detecting the oil stain on the surface of a dropping pill for cigarettes, which comprises the following steps:
(1) preparation of test samples: randomly putting 80g of dropping pills to be tested from a dropping pill production line into a beaker, adding 300mL of 95% hot ethanol, soaking for 10min to remove white oil, filtering and draining by adopting a screen, weighing 20g of ethanol solution containing the white oil, putting the ethanol solution into a separating funnel, adding 25mL of n-hexane and 5g of anhydrous sodium sulfite, violently shaking and mixing for 2min, standing until the solution is transparent, adding 25mL of n-hexane after separating, extracting for 3 times to obtain a mixed solution containing oil stains, and fixing the volume to 50mL by using the n-hexane.
(2) And (3) detecting the absorbance of the test sample: starting an ultraviolet-spectrophotometer, preheating, setting the detection wavelength to 277.10nm, putting n-hexane as a reference solution into a quartz cuvette, and adjusting zero. 1ml of the mixed solution prepared in step (1) was taken and put into a quartz dish to start reading and record the absorbance value, and the average absorbance value of the sample measured 3 times was 0.265.
(3) Calculating the white oil content of the test sample: substituting the sample absorbance value of 0.374 into the standard curve equation y =0.095x +0.029 calculates the white oil content of the sample as: c = (0.265-0.029)/0.095 =2.48 (mg/ml), so the white oil concentration per gram of dropping pill is: c =2.48/20=0.124 (mg/ml).
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (4)
1. A method for detecting the oil stain on the surface of a dropping pill for cigarettes is characterized by comprising the following steps:
preparation of test samples: extracting the dropping pill to be detected by using normal hexane and anhydrous sodium sulfite to obtain a mixed solution containing oil stains;
determining the optimal ultraviolet absorption wavelength: preparing white oil into a solution with the mass fraction of 1% by using n-hexane, taking analytically pure n-hexane as a blank, carrying out wavelength scanning on an ultraviolet-visible spectrophotometer, wherein the scanning wavelength range is 190-400 nm, the scanning speed is medium, the sampling interval is 0.2nm, the slit width is 1.0nm, the thickness of a quartz cuvette is 1cm, and analyzing the absorption peak of an ultraviolet spectrum after scanning for 3 times to determine the optimal absorption wavelength;
drawing a standard curve: preparing a series of standard white oil samples with different concentrations by using n-hexane, sequentially measuring the absorbance values of the samples at the optimal ultraviolet absorption wavelength on an ultraviolet-visible spectrophotometer according to the sequence of the concentration from low to high, and performing linear regression on the absorbance values and the white oil content to obtain a standard curve;
detecting the oil stain content: at the optimal ultraviolet absorption wavelength, putting n-hexane serving as a reference solution into a quartz cuvette, and adjusting zero; and testing the absorbance of the mixed solution, and calculating the surface oil stain quantity of the dropping pill to be tested by using the standard curve.
2. The method for detecting the oil stain on the surface of the dropping pill for cigarettes as claimed in claim 1, wherein the preparation of the test sample is carried out according to the following process: putting 80-100 g of dropping pills to be tested into a beaker, adding 300mL of 95% hot ethanol, soaking for 10-15 min to remove surface white oil, filtering and draining by adopting a screen, weighing 10-50 g of ethanol solution containing the white oil, putting the ethanol solution into a separating funnel, adding 25mL of n-hexane and 5-10 g of anhydrous sodium sulfite, violently shaking and mixing for 1-3 min, standing until the solution is transparent, adding 25mL of n-hexane after separating, and extracting for 2-3 times to obtain the mixed solution containing oil stains.
3. The method for detecting the surface oil stain amount of the dropping pill for cigarette as claimed in claim 1, wherein the optimal absorption wavelength is 277.10 nm.
4. The method for detecting surface oil stain of dropping pills for cigarettes according to claim 1, wherein the detection limit of white oil on the surface of the dropping pills is 0.05mg/g to 0.4 mg/g.
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Cited By (1)
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Application publication date: 20200218 |