Cigar wood packaging material analysis method based on GCMS technology

Abstract

The invention belongs to the field of volatile substance basic detection, and provides a cigar wood packaging material volatile substance analysis method, which comprises: treating a wood to be detected by using a simultaneous distillation extraction method to obtain an extract; mixing the extract with an internal standard substance to obtain an analysis sample; carrying out quantitative and qualitative detection on volatile components of the analysis sample by adopting a GC-MS (Gas Chromatography-Mass Spectrometer) method, and taking detected compounds with the similarity greater than 80 as the analysis sample; the analysis samples are classified according to the differences of the properties and the chemical structures of the compounds, and whether the wood to be detected is cedar or not is judged according to the types and the numbers of terpene substances and ester substances. The method can be used for identifying the cigar wood packaging material, and provides a new research method and thought for the comparison and identification of wood, grading and the research of natural active substances in aromatic wood in the future.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of volatile substance basis detection, and particularly relates to the application of GC / MS technology in analyzing wood volatile substances. BACKGROUND

[0002] The information disclosed in this Background section is only for the purpose of increasing an understanding of the general background of the application and does not necessarily constitute an admission or a recognition that the information forms part of the prior art that is already known in any country in the world.

[0003] Cigar wood generally refers to cedar wood. The unique aroma of cedar wood can play a unique role in the storage and maintenance process of cigar cigarettes, and is a commonly used packaging box raw material for high-end handmade cigars. It is difficult to accurately identify the cedar wood material through sensory methods, especially after the wood material is processed into a special packaging box through a certain process, it is difficult to identify the material by visual inspection, smell and other methods. Through the review of relevant literature, wood is mainly identified by anatomy. By summarizing the macroscopic and microscopic structure characteristics of the wood of each tree species, artificial knowledge or wood retrieval table is used to compare and judge with the existing tree species data in the wood specimen database to identify the wood species. However, this method still has a certain risk of misidentification when the wood is processed. Therefore, it is urgent to establish a wood component analysis method to provide data support for the identification of cigar wood packaging materials. In recent years, some studies have begun to combine the volatile components in wood to assist in wood identification and grade division, which is also of great significance for the study of active substances in aromatic plants. GC / MS technology has the advantages of high sensitivity, fast analysis speed, accurate quantification, wide analysis range, etc., and is a commonly used method for analyzing volatile substances. However, there is currently no method for identifying cedar wood based on GC / MS analysis of wood volatile components. SUMMARY

[0004] In order to solve the above problems, the present application combines the production practice, selects cedar, fir and oak as the test objects which are relatively close to cedar wood, and establishes a wood volatile component analysis method based on GC / MS technology.

[0005] In order to achieve the above purpose, the present application adopts the following technical scheme: The first aspect of the present application provides a cigar wood packaging material quality analysis method based on GC / MS technology, comprising: The wood to be tested is treated by simultaneous distillation extraction to obtain an extract; The extract is mixed with an internal standard to obtain an analysis sample; The volatile components of the analysis sample are quantitatively and qualitatively detected by GC-MS method, and the compounds with a similarity greater than 80 are taken as the analysis sample. According to the differences in the properties and chemical structures of the compounds, the analysis sample is classified, and the types of terpenes and esters are used to determine whether the wood material is cedar wood.

[0006] The present application analyzes the volatile components of four kinds of wood by GC / MS technology, explores the differences of volatile aroma components of different wood, and performs qualitative and quantitative analysis on the aroma components, thereby providing reference and guidance for subsequent wood material identification, volatile substance extraction and analysis.

[0007] In a second aspect, the present application provides a cigar wood packaging material quality analysis system based on GC / MS technology, comprising: a simultaneous distillation extraction device and a GC / MS analyzer.

[0008] Advantages of the present application (1) The present application provides a method for extracting, identifying and qualitatively and quantitatively analyzing volatile substances of wood samples. The volatile substances in wood can be analyzed, thereby providing a research idea for wood identification, grade division and research on volatile active substances.

[0009] (2) The present application first discovers that the types of terpenes and esters in wood can be used to identify whether it is cedar wood, thereby effectively improving the identification efficiency of packaging box raw materials.

[0010] (3) The method of the present application is simple and practical, and is easy to popularize. DETAILED DESCRIPTION

[0011] The accompanying drawings, which form a part of this application, are included to provide a further understanding of the application, and are incorporated in and constitute a part of this application. The embodiments of the present application, and their description, are used to explain the present application and are not intended to limit the present application unduly.

[0012] Figure 1 Fig. 4 is a GC / MS analysis peak chart of four kinds of wood; Figure 2 Fig. 5 is a classification of volatile components of four kinds of wood. DETAILED DESCRIPTION

[0013] It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the present application. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs.

[0014] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or materials used in the present application can be purchased through conventional routes, and are used according to the conventional manner in the art or according to the product instructions, unless otherwise specified. Similarly, the test methods used in the present application are also tested according to the conventional manner in the art or the general method or standard in the industry, unless otherwise specified. In addition, any method and material similar or equivalent to those described can be applied to the method of the present application. The preferred implementation methods and materials described herein are only for demonstration.

[0015] The present application provides a GC / MS technology-based analysis method for the material quality of cigar wood packaging materials, comprising: The wood to be tested is treated by simultaneous distillation extraction to obtain an extract; The extract is mixed with an internal standard to obtain an analysis sample; The volatile components of the analysis sample are quantitatively and qualitatively detected by GC-MS method, and the compounds with a similarity greater than 80 detected are taken as analysis samples; The analysis samples are classified according to the differences in the properties and chemical structures of the compounds, and the types and quantities of terpenes and esters are used to determine whether the material quality of the wood to be tested is cedar wood.

[0016] Preferably, the material quality of the wood to be tested is cedar wood, cypress wood, fir wood, or oak wood. The unique aroma of cedar wood can play a unique role in the storage and maintenance of cigar cigarettes, and is a commonly used packaging box raw material for high-end handmade cigars.

[0017] The conditions of the simultaneous distillation extraction method affect the pretreatment effect, therefore, the conditions of the simultaneous distillation extraction method are studied in the present application, and the specific conditions of the simultaneous distillation extraction method preferably comprise: The wood chips are mixed with water and placed in the left container, heated to micro-boiling and kept; dichloromethane is placed in the right container, the second container is placed in a water bath at 60-65℃, and simultaneous distillation extraction is performed for 2-3 h, after completion, the dichloromethane bottle is taken out, anhydrous sodium sulfate is added to the bottle for drying, and rotary evaporation is performed to 0.8-1.2 mL, thereby improving the extraction effect of volatile components.

[0018] The type and concentration of the internal standard affect the accuracy and reliability of the detection, therefore, the type and concentration of the internal standard are studied in the present application, and the internal standard is preferably phenethyl acetate solution with a concentration of 1.0-1.2 mg / L, thereby improving the accuracy and reliability of the detection.

[0019] The conditions of the GC-MS method can affect the accuracy of detection, therefore, the conditions of the GC-MS method are researched in the application, preferably, the specific conditions of the GC-MS method analysis include: GC conditions: flexible quartz capillary column (HP-5MS, 30 m x 250 pm x 25 pm); the carrier gas is ultrapure helium; the flow rate is 1.0-1.5 mL·min -1 ; the injection port temperature is 250-260 DEG C; the injection amount is 1-2 mu L; the split ratio is 40-45:1; the programmed temperature is: the initial temperature is 40 DEG C, and the temperature is kept for 1 min; then the temperature is increased to 100 DEG C at the rate of 10 DEG C·min -1 , the temperature is increased to 140 DEG C at the rate of 20 DEG C·min -1 , and the temperature is kept for 2 min; then the temperature is increased to 250 DEG C at the rate of 20 DEG C·min -1 , and the temperature is kept for 3 min.

[0020] MS conditions: the transfer line temperature is 280-290 DEG C; the ion source temperature is 230-240 DEG C; the quadrupole temperature is 150-160 DEG C; the electromagnetic source is EI; the ion source is EI; the ionization energy is 70-80 eV; the scanning mass range is 15-500 amu; the mass spectrum scanning mode is full scan (SCAN); the solvent delay is 4 min, so as to improve the detection accuracy.

[0021] The application ensures the accuracy of subsequent identification by screening the sample. Preferably, the detected volatile components are analyzed by mass spectrometry and NIST2020 spectral library retrieval, and the compounds with a matching factor greater than 80 are used as analysis samples, so that better identification accuracy can be obtained.

[0022] The application classifies the compounds, and finds that different woods have special terpene substances and ester substances. Preferably, the compounds are classified into 10 categories, namely alcohol, phenol, ether, aldehyde, alkaloid, acid, terpene, ketone, alkane and ester, so as to facilitate subsequent identification.

[0023] The application establishes the identification conditions of the wood based on the classification of volatile components, preferably, if the terpene substances are greater than 25 and the ester substances are greater than 15, then it is determined as cedar wood, so as to realize accurate identification of cedar wood.

[0024] Preferably, the peak area normalization method is used for quantitative analysis, so as to improve the detection accuracy.

[0025] The application will be further described in detail in combination with specific examples, it should be pointed out that the specific examples are an explanation of the application rather than a limitation.

[0026] The application analyzes the aroma substances of the treated wood by using GC / MS technology, and qualitatively and quantitatively analyzes the data by using different analysis methods, and classifies the substances in the wood.

[0027] Example 1 The application of the volatile substance determination method in determining the volatile substances in four kinds of wood (oak wood, cypress wood, fir wood and cedar wood).

[0028] The specific steps are as follows: (1) Using the method of simultaneous distillation extraction, 10.000 g of wood chips of four kinds of wood is taken and placed in a 500 mL round-bottom flask, 200 mL of distilled water is added, and an electric heating jacket is used for heating to maintain a slight boiling; 50 mL of dichloromethane is taken and placed in a 500 mL round-bottom flask, and heated with a water bath to maintain the water bath temperature at 60℃, and the distillation extraction is carried out for 2 h, then the dichloromethane bottle is taken out, 1.0 g of anhydrous sodium sulfate is added to the bottle and dried for 1 h, and rotary evaporation is carried out at 50℃ water bath under normal pressure to about 1 mL, and 10 μL of internal standard (phenyl ethyl acetate solution 1.0 mg / L) is added.

[0029] (2) The extracted volatile substances are detected by GC-MS according to the above method and parameter setting.

[0030] GC conditions: flexible quartz capillary column (HP-5MS, 30 m x 250 μm x 25 μm); carrier gas is ultrapure helium; flow rate is 1.0 mL·min -1 ; the inlet temperature is 250℃; the sample size is 1 μL; the split ratio is 40:1; the programmed temperature is: the initial temperature is 40℃, and is maintained for 1 min; then increased to 100℃ at 10℃·min -1 , increased to 140℃ at 20℃·min -1 , maintained for 2 min; then increased to 250℃ at 20℃·min -1 , maintained for 3 min.

[0031] MS conditions: transfer line temperature 280℃; ion source temperature 230℃; quadrupole temperature 150℃; electromagnetic source EI; ion source EI; ionization energy 70 eV; scanning mass range 15~500 amu; mass spectrum scanning mode: full scan (SCAN); solvent delay 4 min.

[0032] (3) Qualitative analysis: the detected volatile components are analyzed by mass spectrometry and searched in NIST2020 library, and the matching factor is greater than 80; quantitative analysis: peak area normalization method.

[0033] Experimental Example 1: Types of volatile substances Analysis revealed peak patterns of volatile components in four types of wood obtained by GC-MS detection, as shown below. Figure 1 As shown, there are 102 species of cedar, 100 species of cypress, 65 species of oak, and 55 species of fir, which are relatively similar to the characteristic volatile substances in the literature.

[0034] Experimental Example 2: Classification of Volatile Substances like Figure 2 As shown, compounds with a similarity greater than 80 were analyzed and classified into 10 categories based on their properties and differences in chemical structure. Specifically, cedar wood contained 3 alcohols, 2 phenols, 8 ethers, 9 aldehydes, 1 alkaloid, 1 acid, 37 terpenes, 11 ketones, 10 alkanes, and 22 esters; cypress wood contained 28 alcohols, 3 phenols, 3 ethers, 1 aldehyde, 2 acids, 47 terpenes, 4 ketones, 3 alkanes, and 8 esters; fir wood contained 10 alcohols, 2 aldehydes, 25 terpenes, 3 ketones, 6 alkanes, and 7 esters; and oak wood contained 9 alcohols, 3 phenols, 1 ether, 7 aldehydes, 4 acids, 6 terpenes, 9 ketones, 5 alkanes, and 19 esters.

[0035] Cedar, cypress, and fir contain significantly more terpenes than oak. Cedar and oak contain more esters than cypress and fir. Fir contains the fewest volatile compounds; phenols, ethers, alkaloids, and acids were not detected in fir wood. Therefore, the variety and quantity of terpenes and esters can serve as the main analytical direction and basis for determining the differences between cedar and the other three types of wood.

[0036] Based on this, the present invention further quantifies the criteria for determining cedar wood as follows: if there are more than 25 kinds of terpenes and more than 15 kinds of esters, it is determined to be cedar wood; otherwise, it is determined to be non-cedar wood.

[0037] Experiment Example 3: Experiment on the identification of wood species Take 25 pieces each of cedar, cypress, fir, and oak, and analyze their volatile components according to the above method. The judgment is based on the standard that "there are more than 25 kinds of terpenes and more than 15 kinds of esters". The results show that the accuracy rate is 98%.

[0038] Therefore, it can be seen that whether a piece of wood is cedar can be identified based on the types and quantities of terpenes and esters in it. The method of the present invention effectively improves the efficiency and accuracy of identifying raw materials for packaging boxes.

[0039] The above merely provides the preferred embodiments of the present application, and is not used to limit the present application. For those skilled in the art, the present application can have various modifications and changes. Any modifications, equivalent replacements, improvements, etc. made within the principles and technical scope of the present application shall fall into the scope of the present application.

Claims

1. A method for analyzing the material composition of wooden cigar packaging materials based on GC / MS technology, characterized in that, include: The wood to be tested was treated with a simultaneous distillation-extraction method to obtain the extract; The extract was mixed with an internal standard to obtain the analytical sample; The volatile components of the analytical samples were quantitatively and qualitatively detected by GC-MS, and the compounds with a similarity greater than 80 were selected as analytical samples. The analytical samples are classified according to the differences in the properties and chemical structures of the compounds, and the type and quantity of terpenes and esters are used to determine the material of the wood to be tested.

2. The method for analyzing the material composition of cigar wood packaging based on GC / MS technology as described in claim 1, characterized in that, The wood to be tested is made of cedar, cypress, fir, or oak.

3. The method for analyzing the material composition of cigar wood packaging materials based on GC / MS technology as described in claim 1, characterized in that, The specific conditions for the simultaneous distillation-extraction method include: Take wood chips and water, place them in the left container, heat to a gentle boil and maintain; take dichloromethane and place it in the right container, place the second container in a water bath at 60 ℃-65 ℃, and distill and extract for 2-3 h. After completion, remove the dichloromethane bottle, add anhydrous sodium sulfate to the bottle for drying, and rotary evaporate to 0.8-1.2 mL to obtain the product.

4. The method for analyzing the material composition of cigar wood packaging materials based on GC / MS technology as described in claim 1, characterized in that, The internal standard is a phenethyl acetate solution with a concentration of 1.0-1.2 mg / L.

5. The method for analyzing the material composition of cigar wood packaging based on GC / MS technology as described in claim 1, characterized in that, The specific conditions for the GC-MS analysis include: GC conditions: Flexible quartz capillary column (HP-5MS, 30 m × 250 µm × 25 µm); ultrapure helium as carrier gas; flow rate 1.0–1.5 mL / min. -1 Injector temperature: 250-260℃; Injection volume: 1-2 μL; Split ratio: 40-45:1; Temperature program: Initial temperature 40℃, hold for 1 min; then increase at 10℃ / min. -1 Rise to 100℃, 20℃·min -1 Raise to 140℃ and hold for 2 minutes; then increase by 20℃·min. -1 Raise the temperature to 250℃ and maintain it for 3 minutes; MS conditions: transfer line temperature 280-290℃; ion source temperature 230-240℃; quadrupole temperature 150-160℃; electromagnetic source EI; ion source EI; ionization energy 70-80 eV; scan mass range 15~500 amu; mass spectrometry scan mode: full scan (SCAN); solvent delay 4 min.

6. The method for analyzing the material composition of cigar wood packaging materials based on GC / MS technology as described in claim 1, characterized in that, The detected volatile components were analyzed by mass spectrometry and searched in the NIST 2020 spectral library. Compounds with a matching factor greater than 80 were used as analytical samples.

7. The method for analyzing the material composition of cigar wood packaging materials based on GC / MS technology as described in claim 1, characterized in that, Compounds are classified into 10 categories: alcohols, phenols, ethers, aldehydes, alkaloids, acids, terpenes, ketones, alkanes, and esters.

8. The method for analyzing the material composition of cigar wood packaging based on GC / MS technology as described in claim 1, characterized in that, If there are more than 25 terpenes and more than 15 esters, it is identified as cedarwood.

9. The method for analyzing the material composition of cigar wood packaging materials based on GC / MS technology as described in claim 1, characterized in that, Quantitative analysis was performed using the peak area normalization method.

10. A material analysis system for cigar wood packaging materials based on GC / MS technology, comprising: Simultaneously, a distillation and extraction device and a GC / MS analyzer were used.

Images