CN104597155A - Quality control method for agilawood - Google Patents
Quality control method for agilawood Download PDFInfo
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- CN104597155A CN104597155A CN201510012278.5A CN201510012278A CN104597155A CN 104597155 A CN104597155 A CN 104597155A CN 201510012278 A CN201510012278 A CN 201510012278A CN 104597155 A CN104597155 A CN 104597155A
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Abstract
The invention discloses a quality control method for agilawood. The quality control method comprises the following steps: respectively detecting different grades of agilawood products, thereby correspondingly obtaining the composition of volatile components of all the grades of products, the average value of the contents and a standard deviation, and establishing a quality control standard; and comparing the average value of the contents of volatile components of unknown-grade products with the established quality control standard and judging the grade. The quality control method disclosed by the invention applies fast pyrolysis-gas chromatography and mass spectrometry analysis in quality control of the agilawood, and has the advantages of fastness, convenience, high efficiency, high sensitivity, low detection limit, good reproducibility and the like.
Description
Technical field
The invention belongs to fragrant product quality of production analysis & control field, be specifically related to the method for quality control of a kind of agalloch eaglewood.
Background technology
Fragrant product have long history in China.From ancient times to the present, people are just making great efforts to improve the method using spices, fragrant product always, on the one hand the value of spices can be utilized more fully, also convenient on the other hand.The kind of the present fragrant product of China is very abundant.Specifically, according to using the scentetd mode of fragrant product to be divided into: burn joss sticks, Tu Xiang, fragrant soup, wear fragrant etc.; Then fragrant block, face powder, herb pieces, sesame oil and perfume etc. can be divided into according to fragrant product form.Fragrant, the last perfume of lobe, line spices, sleeping perfume (or spice), fragrant tower, pomander, incense coil etc. then can be divided into according to fragrant product shape.Different kinds and form, shape all have different starting material, production technology and using method.Burn joss sticks in actual production, life, line spices remain most popular, as Fo Dao fragrant, tea ceremony perfume etc.
There is the beneficiating ingredient of tranquilizing and allaying excitement, pleasant mental and body in fragrant product combustion process, but also have many to healthy harmful material, common are metal pollutant and the volatile organic composition such as lead (Pb), cadmium (Cd).There is Buddhist monk's contact and imbedibility disease in China's many ground temple, reason of searching to the bottom is caused by a large amount of fake and forged fragrant product of Long Term Contact.
Existing fragrant product are produced and are lacked for the effective quality analysis of finished product and method of quality control.Starting material, auxiliary material, adjuvant, bonding agent etc. that current most standard is just produced for fragrant product.Part economizes grade standard to be had and relates to metal pollutant and formaldehyde, but not for the examination criteria of volatile organic compounds (VOCs) and polynuclear aromatics compounds (PAHs).And these volatile organic compounds (VOCs) and polynuclear aromatics compounds (PAHs) are only one of the basic source and pathogenic basic reason of fragrance.
The existing industry for fragrant quality and drug in some provinces standard ubiquity operating process complexity, the shortcomings such as analysis time is long, and sensitivity is low.In addition, existing standard just for the raw-material standard in fragrant product production, lacks the direct-detection to fragrant product products of combustion.As the national standard of " notice about carrying out and implementing 3 national standards such as " series products safety general technical conditions of burning incense " " and " series products safety general technical conditions of burning incense ", " series products objectionable impurities of burning incense method of testing " and " venue for religious activities and tourist quarters burn incense safety standard " in Anhui Province, be all the starting material for producing and using method.Therefore, it is extremely important and necessary for setting up the direct quality standard for fragrant product products of combustion.
Regrettably, the method to the burning of fragrant product and efficient, the quick detection of pyrolysis product is still lacked at present.Conventional detection is still the sensation relying on and hear fragrant teacher.
Summary of the invention
The object of the present invention is to provide the method for quality control of a kind of agalloch eaglewood.
For achieving the above object, present invention employs following technical scheme:
Step one, utilize fast pyrogenation-gas chromatography combined with mass spectrometry analysis to detect respectively to the product of agalloch eaglewood different brackets, obtain agalloch eaglewood quality control with reference to the content of component in corresponding grade products;
The condition of described fast pyrogenation is: pyrolysis temperature is 100 DEG C ~ 800 DEG C, and pyrolysis time is 0.1min ~ 20min;
The condition of work of described gas chromatography is: carrier gas is the helium of flow velocity 0.1mL/min ~ 4.0mL/min, and split ratio is 0 ~ 500:1; Heating schedule is: initial temperature is 40 DEG C ~ 80 DEG C, and keep 0min ~ 6min, then with the ramp to 180 DEG C of 0.1 DEG C/min ~ 10 DEG C/min, then with the ramp to 280 DEG C of 5 DEG C/min ~ 15 DEG C/min, and keep 0min ~ 10min, again with the ramp to 310 DEG C of 5 DEG C/min ~ 15 DEG C/min, and keep 0min ~ 10min;
Described mass spectrographic condition of work is: adopt EI source, positive ion detection, electron energy is 70eV ~ 120eV, ion source temperature is 200 DEG C ~ 250 DEG C, single level Four bar temperature is 130 DEG C ~ 200 DEG C, scan mode is full scan mode, electron-multiplier voltage is 1070V ~ 3120V, and solvent delay is 0min ~ 20min;
Step 2, repetition step one at least three times, then calculate agalloch eaglewood quality control with reference to the content mean value of component in corresponding grade products and standard deviation, and the content range determined using described mean value and standard deviation is as the quality control standard of the corresponding grade products of agalloch eaglewood;
Step 3, adopt the detection method same with step one to carry out at least three times to agalloch eaglewood grade products undetermined to detect, obtain the average content of agalloch eaglewood grade products quality control reference undetermined component;
Step 4, grade products quality control undetermined for agalloch eaglewood to be compared with reference to the average content of component and quality control standard, if the average content of agalloch eaglewood grade products undetermined quality control reference component all reaches the quality control standard of a certain grade products, then judge that described grade products undetermined is as described a certain grade.
Described detection specifically comprises the following steps:
Step 1, agalloch eaglewood to be detected is ground rear mistake 80 ~ 120 mesh sieve, extracting screen underflow is as sample;
Step 2, sample described in step 1 is placed in the pyrolysis cup of pyrolysis analyzer, and while pyrolysis sample, adopt gas chromatograph-mass spectrometer (GCMS) to detect the sample in pyrolysis cup, according to the chromatographic data detected and mass spectrometric data, the composition of calculation sample volatile ingredient and content.
Described content is relative content and absolute content, and described relative content adopts area normalization method to calculate, and the computing method of described absolute content are: the ratio of the peak area that each volatile ingredient is corresponding and internal standard compound peak area is multiplied by the quality of internal standard compound again.
Described internal standard compound is 1,3,5-trimethylbenzene, 1,3,5-triethylbenzene, 1,3,5-triisopropylbenzene, 1,3,5-tri-butyl benzene, 1,3,5-trimethoxy-benzene or 1,3,5-triethoxy benzene.
Described agalloch eaglewood quality control reference group is divided into 3,4-dihydroxy dihydroagarofuran, agarofuran and linalool.
In the quality control standard of the corresponding grade products of relative content agalloch eaglewood be:
3,4-dihydroxy dihydroagarofuran: >=0.483% is high-class product; >=0.477% is Grade A; >=0.471% is goods of inferior quality; < 0.471% is unacceptable product;
Agarofuran: >=1.876% is high-class product; >=1.870% is Grade A; >=1.864% is goods of inferior quality; < 1.864% is unacceptable product;
Linalool: >=5.121% is high-class product; >=5.115% is Grade A; >=5.109% is goods of inferior quality; < 5.109% is unacceptable product.
Beneficial effect of the present invention is embodied in:
The present invention is directly for the quality control of finished product perfume (or spice), traditional quality control to fragrant product is mainly for the use of the starting material, auxiliary material, bonding agent, adjuvant etc. in fragrant product production, but in actual use, even if use the starting material of natural environmental-protective, also be difficult to ensure that it does not discharge poisonous and harmful substances in combustion, polynuclear aromatics compounds as carcinogenic in height.This is because high temperature during burning makes starting material there occurs pyrolytic reaction, harmless raw material pyrolysis becomes harmful volatile organic compounds etc.Therefore, quality control only for starting material etc. in actual production, R&D process is far from being enough, the present invention is just for this general difficulty, propose a kind of method of quality control based on volatile ingredient in the use of fragrant product (agalloch eaglewood) reality, the quality grade of fragrant product can be reflected intuitively, fast and accurately, be conducive to the research and development accelerating fragrant product, and improve quality and the production efficiency of fragrant product, in addition, method of quality control of the present invention is easy to standardization, significantly reduces the interference of subjective factor.
In addition, the present invention also has the following advantages:
1, the Qualitative and quantitative analysis that method of quality control of the present invention is researched and developed fragrant product based on PY-GC-MS technology, production run carries out data result in quality analysis and quality control directly completes by software, as long as operate according to experimental standard, all can obtain the extraordinary result of reappearance, be easy to standardization; And effectively can judge the volatile constituent in fragrant product to the qualitative examination of chromatographic peak, to the compatibility of novel fragrant product and and the research and development of blending very helpful.
2, fast pyrogenation-Gc-ms technology is applied in the quality control of finished product perfume (or spice) by the present invention, have quick, convenient, efficient, highly sensitive, detectability is low, high repeatability and other advantages.Fast pyrogenation-Gc-ms technology (PY-GC-MS) is a kind of technology of efficient detection volatile constituent, has high heating rate, thermal cracking temperature and time adjustable, the technical advantage such as volatile constituent fast transfer or cooling.When adopting PY-GC-MS to carry out thermal cracking test to the fragrant product sample of difference, thermal cracking gas directly can carry out on-line analysis by GC-MS, determines that its thermal cracking generates the contamination of product, and carries out analysis and comparison to result.PY-GC-MS technology is separated with gas chromatography powerful when integrating accurate temperature controlling, the control of pyrolysis oven, analysis ability and mass spectrographic high sensitivity, the large advantage of low detection limit three, all fragrant temperature and times in the actual use procedure of fragrant product can be covered, ensure that the method can maximum simulating practical service environment.Adopt the method, every batch sample detects only needs about 1 hours, saves human and material resources, financial resources, can reach the object detected fast, improve work efficiency.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated.
Embodiment
(1) composition of fragrant product volatile ingredient and content detection
Step one, agalloch eaglewood face powder to be detected is ground rear mistake 80 mesh sieve, extracting screen underflow is as sample;
Sample described in the step one of step 2, precise 1.00mg (± 0.02mg), be placed in the pyrolysis cup of pyrolysis analyzer, while pyrolysis, adopt gas chromatograph-mass spectrometer (GCMS) to detect the sample in pyrolysis cup, according to the chromatographic data detected and mass spectrometric data, the composition of calculation sample volatile ingredient, relative content and absolute content; Described relative content adopts area normalization method to calculate, and the computing method of described absolute content are: the ratio of the peak area that each volatile ingredient is corresponding and internal standard compound 1,3,5-trimethylbenzene peak area is multiplied by the quality of internal standard compound again;
Pyrologger in the present embodiment adopts the PY2020is of Frontiers, and the condition of work of pyrolysis is: pyrolysis temperature is 220 DEG C, and pyrolysis time is 0.20min;
Chromatogram: detect and adopt Agilent 7890A/5975C;
1. analytical column is HP-5MS fused-silica capillary column (30m × 0.25id × 0.25 μm);
2. carrier gas: helium, flow velocity is 1.0mL/min;
3. sample size 1mg, input mode is split sampling, and split ratio is 100:1;
4. injector temperature 290 DEG C, transmission line temperature 300 DEG C;
5. temperature programme, initial temperature is 40 DEG C, keeps 3min, then rises to 180 DEG C with 4 DEG C/min, then rise to 280 DEG C with 10 DEG C/min, keeps 4min, then rises to 310 DEG C with 10 DEG C/min, keeps 4min;
Mass spectrum:
1. EI source, positive ion detects, and electron energy is 70eV;
2. ion source temperature 230 DEG C, single level Four bar temperature 150 DEG C;
3. scan mode is full scan mode;
4. electron-multiplier voltage 1070V, solvent delay 1.5min;
Step 3, step 23 times is repeated to sample described in step one, the mean value of calculation sample volatile component content.
(2) foundation of quality control standard
Detect respectively according to the product of method to agalloch eaglewood different brackets (high-class product, Grade A, goods of inferior quality) of step one to step 3, obtain the composition of the volatile ingredient of each grade products and the mean value of content and standard deviation accordingly, select 3 in agalloch eaglewood volatile ingredient, 4-dihydroxy dihydroagarofuran, agarofuran, linalool are as reference component, with with reference to the content mean value of component in each grade products and standard deviation determination content range, and as the quality control standard of corresponding grade products.Detect the mean value that obtains and standard deviation as follows:
3,4-dihydroxy dihydroagarofuran: 0.486% ± 0.03 (high-class product); 0.480% ± 0.03 (Grade A); 0.474% ± 0.03 (goods of inferior quality);
Agarofuran: 1.879% ± 0.03 (high-class product); 1.873% ± 0.03 (Grade A); 1.867% ± 0.03 (goods of inferior quality);
Linalool: 5.124% ± 0.03 (high-class product); 5.118% ± 0.03 (Grade A); 5.112% ± 0.03 (goods of inferior quality);
Describe in the mode of the minimum reaching a certain grade according to the quality control standard that testing result obtains.Analyze through taking statistics with the result of artificial evaluation rank, grade result of determination indifference.
(3) grade judges
Adopt and with step 2, three same methods in (one), grade agalloch eaglewood product undetermined is detected, obtain the average content of grade agalloch eaglewood product undetermined reference component; Then the average content of grade agalloch eaglewood product reference component undetermined and agalloch eaglewood quality control standard are compared, if grade agalloch eaglewood product undetermined all reaches the quality control standard of a certain grade agalloch eaglewood with reference to component concentration, then judge that grade agalloch eaglewood product undetermined is as described a certain grade.In this detection sample, identifiable peak is 44, and all the other peaks are moisture, inert gas etc.; Identifiable volatile constituent and retention time thereof list in table 1; Retention time and peak area Agilent Chemstation calculate, and the method for relative content area normalization calculates;
The composition of volatile ingredient and content in table 1 agalloch eaglewood
Note: reference group is divided into 10.3,4-Dihydroxydihydgaroaroiuran (3,4-dihydroxy dihydroagarofuran) t
r=37.632; 17. α-Agarofuran (agarofuran) t
r=41.547; 31.Linalool (linalool) t
r=44.514.
Carry out experimental study to the precision of the inventive method, reappearance and stability, result is as follows.
1, Precision Experiment: 1 part, the sample getting the embodiment of the present invention, according to the method continuous sample introduction 7 times of embodiment, is greater than 42 chromatographic peak (CO of 0.5% to relative peak area
2and internal standard compound is disregarded) analyze, the RSD of its relative retention time and relative peak area, respectively between 0% ~ 0.09% and 0.03% ~ 0.34%, illustrates that the inventive method precision is good.
2, reappearance experiment: 7 parts, the different samples getting same batch, operate according to the method for embodiment, are compared by 7 groups of chromatograms.The relative retention time of 42 chromatographic peaks and the RSD of relative peak area are respectively between 0% ~ 0.21% and 0.19% ~ 0.49% as a result, illustrate that the inventive method reappearance is good.
3, stability experiment: get 1 part, the sample prepared, respectively 0,1,3,5,10,24,48h sample introduction measures, the relative retention time of 42 chromatographic peaks and the RSD of relative peak area are all less than 1% as a result, and it is stable for illustrating that the inventive method measures in 48h.
Claims (6)
1. a method of quality control for agalloch eaglewood, is characterized in that: comprise the following steps:
Step one, utilize fast pyrogenation-gas chromatography combined with mass spectrometry analysis to detect respectively to the product of agalloch eaglewood different brackets, obtain agalloch eaglewood quality control with reference to the content of component in corresponding grade products;
The condition of described fast pyrogenation is: pyrolysis temperature is 100 DEG C ~ 800 DEG C, and pyrolysis time is 0.1min ~ 20min;
The condition of work of described gas chromatography is: carrier gas is the helium of flow velocity 0.1mL/min ~ 4.0mL/min, and split ratio is 0 ~ 500:1; Heating schedule is: initial temperature is 40 DEG C ~ 80 DEG C, and keep 0min ~ 6min, then with the ramp to 180 DEG C of 0.1 DEG C/min ~ 10 DEG C/min, then with the ramp to 280 DEG C of 5 DEG C/min ~ 15 DEG C/min, and keep 0min ~ 10min, again with the ramp to 310 DEG C of 5 DEG C/min ~ 15 DEG C/min, and keep 0min ~ 10min;
Described mass spectrographic condition of work is: adopt EI source, positive ion detection, electron energy is 70eV ~ 120eV, ion source temperature is 200 DEG C ~ 250 DEG C, single level Four bar temperature is 130 DEG C ~ 200 DEG C, scan mode is full scan mode, electron-multiplier voltage is 1070V ~ 3120V, and solvent delay is 0min ~ 20min;
Step 2, repetition step one at least three times, then calculate agalloch eaglewood quality control with reference to the content mean value of component in corresponding grade products and standard deviation, and the content range determined using described mean value and standard deviation is as the quality control standard of the corresponding grade products of agalloch eaglewood;
Step 3, adopt the detection method same with step one to carry out at least three times to agalloch eaglewood grade products undetermined to detect, obtain the average content of agalloch eaglewood grade products quality control reference undetermined component;
Step 4, grade products quality control undetermined for agalloch eaglewood to be compared with reference to the average content of component and quality control standard, if the average content of agalloch eaglewood grade products undetermined quality control reference component all reaches the quality control standard of a certain grade products, then judge that described grade products undetermined is as described a certain grade.
2. the method for quality control of a kind of agalloch eaglewood according to claim 1, is characterized in that: described detection specifically comprises the following steps:
Step 1, agalloch eaglewood to be detected is ground rear mistake 80 ~ 120 mesh sieve, extracting screen underflow is as sample;
Step 2, sample described in step 1 is placed in the pyrolysis cup of pyrolysis analyzer, and while pyrolysis sample, adopt gas chromatograph-mass spectrometer (GCMS) to detect the sample in pyrolysis cup, according to the chromatographic data detected and mass spectrometric data, the composition of calculation sample volatile ingredient and content.
3. the method for quality control of a kind of agalloch eaglewood according to claim 2, it is characterized in that: described content is relative content and absolute content, described relative content adopts area normalization method to calculate, and the computing method of described absolute content are: the ratio of the peak area that each volatile ingredient is corresponding and internal standard compound peak area is multiplied by the quality of internal standard compound again.
4. the method for quality control of a kind of agalloch eaglewood according to claim 3, is characterized in that: described internal standard compound is 1,3,5-trimethylbenzene, 1,3,5-triethylbenzene, 1,3,5-triisopropylbenzene, 1,3,5-tri-butyl benzene, 1,3,5-trimethoxy-benzene or 1,3,5-triethoxy benzene.
5. the method for quality control of a kind of agalloch eaglewood according to claim 1, is characterized in that: described agalloch eaglewood quality control reference group is divided into 3,4-dihydroxy dihydroagarofuran, agarofuran and linalool.
6. the method for quality control of a kind of agalloch eaglewood according to claim 5, is characterized in that: in the quality control standard of the corresponding grade products of relative content agalloch eaglewood be:
3,4-dihydroxy dihydroagarofuran: >=0.483% is high-class product; >=0.477% is Grade A; >=0.471% is goods of inferior quality; < 0.471% is unacceptable product;
Agarofuran: >=1.876% is high-class product; >=1.870% is Grade A; >=1.864% is goods of inferior quality; < 1.864% is unacceptable product;
Linalool: >=5.121% is high-class product; >=5.115% is Grade A; >=5.109% is goods of inferior quality; < 5.109% is unacceptable product.
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Cited By (6)
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| CN105136937A (en) * | 2015-09-18 | 2015-12-09 | 西安科技大学 | Magnolol and honokiol quick detection method |
| CN106053645A (en) * | 2016-06-01 | 2016-10-26 | 中国广州分析测试中心 | Method for identifying authenticity of agilawood |
| CN106198791A (en) * | 2016-06-28 | 2016-12-07 | 中山出入境检验检疫局检验检疫技术中心 | Lignum Aquilariae Resinatum tetrol and the method for benzylacetone in a kind of Lignum Aquilariae Resinatum of mensuration simultaneously |
| CN108760921A (en) * | 2018-05-29 | 2018-11-06 | 云南中烟工业有限责任公司 | A kind of analysis method of cigarette agalloch eaglewood flue gas volatile chemical component |
| CN112630339A (en) * | 2020-12-18 | 2021-04-09 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN114112951A (en) * | 2021-11-17 | 2022-03-01 | 广东省科学院动物研究所 | Method for identifying insect-leaked agilawood with high spectrum |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136937A (en) * | 2015-09-18 | 2015-12-09 | 西安科技大学 | Magnolol and honokiol quick detection method |
| CN106053645A (en) * | 2016-06-01 | 2016-10-26 | 中国广州分析测试中心 | Method for identifying authenticity of agilawood |
| CN106053645B (en) * | 2016-06-01 | 2019-04-05 | 中国广州分析测试中心 | A method of identifying the agalloch eaglewood true and false |
| CN106198791A (en) * | 2016-06-28 | 2016-12-07 | 中山出入境检验检疫局检验检疫技术中心 | Lignum Aquilariae Resinatum tetrol and the method for benzylacetone in a kind of Lignum Aquilariae Resinatum of mensuration simultaneously |
| CN106198791B (en) * | 2016-06-28 | 2018-09-11 | 中山出入境检验检疫局检验检疫技术中心 | Method that is a kind of while measuring agalloch eaglewood tetrol and benzylacetone in agalloch eaglewood |
| CN108760921A (en) * | 2018-05-29 | 2018-11-06 | 云南中烟工业有限责任公司 | A kind of analysis method of cigarette agalloch eaglewood flue gas volatile chemical component |
| CN108760921B (en) * | 2018-05-29 | 2021-03-16 | 云南中烟工业有限责任公司 | Analysis method for volatile chemical components of agilawood smoke for cigarettes |
| CN112630339A (en) * | 2020-12-18 | 2021-04-09 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN112630339B (en) * | 2020-12-18 | 2022-07-26 | 广东省测试分析研究所（中国广州分析测试中心） | Method for simultaneously and quantitatively measuring 4 blood-entering components in agilawood alcohol extract |
| CN114112951A (en) * | 2021-11-17 | 2022-03-01 | 广东省科学院动物研究所 | Method for identifying insect-leaked agilawood with high spectrum |
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