CN109900824A - The measuring method of borneol absolute content in a kind of Blumea balsamifera - Google Patents
The measuring method of borneol absolute content in a kind of Blumea balsamifera Download PDFInfo
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Abstract
The invention belongs to medicinal material chemical composition analysis technical fields, the measuring method of borneol absolute content specially in Blumea balsamifera.The method of the present invention includes: to be made into series standard solution with borneol standard items, establishes standard curve by automatic HS GC-Mass Spectrometry；The borneol content in Blumea balsamifera leaf powder is measured again, and the absolute content of borneol in Blumea balsamifera is directly checked in from standard curve.The present invention, which compensates for existing method method, can only obtain the shortcoming of borneol relative amount, can in more actual response Blumea balsamifera sample borneol content.This method is small to sample requirements, and solvent is not used in the measurement of Blumea balsamifera sample, environmentally friendly.It is examined using F and t method of inspection is compared the measurement result of the method with traditional steam distillation-gas-chromatography-flame ionization ditector method, the result shows that, for the assay of borneol, two methods do not differ significantly, and illustrate that this method can be used for Blumea balsamifera medicinal material or the quality control of its extract.
Description
Technical field
The invention belongs to medicinal material chemical composition analysis technical fields, and in particular to the measurement of borneol absolute content in Blumea balsamifera
Method.
Background technique
Blumea balsamifera is composite family (Asteraceae) Blumea balsamifera platymiscium, and the field of Chinese medicines is also known as Balsamiferou Blumea Herb, borneol Chinese mugwort etc., can
Make Chinese herbal medicine or fragrance uses.Blumea balsamifera main product is in Guangxi, Guizhou and other places.Currently, Blumea balsamifera is one of ten seedlings medicine of Guizhou Province.
From the point of view of having the report result of the research to Blumea balsamifera chemical component, flavones and volatile oil are what composite family Blumea balsamifera belonged to
Main component.Flavone compound has: flavanones, luteolin, 3,5,3 '-trihydroxies -4 '-methoxyl group flavanone, 3,
5,3 '--7,4 '-dimethoxy flavanones of trihydroxy, 3,5,3 '-trihydroxies -7,4 '-dimethoxy flavone, 5,7,3 ', 5 ' -
(research [J] of flavone compound in Deng Qinying, Li Xuan, Yang Shunjuan Blumea balsamifera such as tetrahydroxy flavanone, QuercetinWave spectrum Learn magazine, 1996,13 (5): 447.).Volatile oil can be divided into monoterpenes and sequiterpene etc., and monoterpene has borneol, carypohyllene, camphor tree
Brain, linalool etc., sequiterpene have blumealactone, in addition also containing cupreol, stigmasterol (Zhao Jinhua, Kang Hui, Yao Guanghui,
Zeng Weizhen Blumea balsamifera chemical constitution study [J]Chinese herbal medicine, 2007,38 (3): 350.).
It is most containing borneol in Blumea balsamifera leaf and stem, thus be the important plant material for extracting natural L-Borneol.Modern pharmacodynamics
Studies have shown that the borneol in Blumea balsamifera can inhibit the growth of various bacteria, it is the raw material of many precious Chinese patent medicines in China.In recent years
Come, it is available on the market to have the vertical refreshing dripping pill of pharynx, (official's tinkling of pieces of jade such as compound Common Goldenrod Herb spray with drug of the oil for primary raw material that end
It is bright, Pang Yuxin, wangdan, name of the country race special medicinal material Blumea balsamifera progress [J] in Zhang Yingbo, Wu KongyuanPlant genetic resources Report, 2012,13 (4): 695.).
The Research Literature discovery in relation to Blumea balsamifera volatile component in recent years is consulted, majority research is to pass through red, orange, green, blue, yellow (ROGBY)
The relative quantification measurement of borneol is carried out in conjunction with area normalization method.It is a small amount of that absolute content measurement is carried out by calibration curve method
Document, and be measured again after extracting borneol in Blumea balsamifera by solvent, and lack knot obtained by different measuring methods
Direct comparison between fruit.
Week, glad wait obtained volatile oil from Luodian county county Blumea balsamifera blade, by GC-MS Analysis, examined altogether
41 kinds of substances are measured, quantitative manner is area normalization method, and acquired results are relative amount (Zhou Xin, the Yang little Sheng of borneol etc.
The gas phase of Blumea balsamifera chemical composition of volatile oil-mass spectral analysisAnalysis test journal, 2001,20 (5): 75.).
Wang Yuanhui etc. is analyzed by gas chromatography-mass spectrography, comparative studies Various Seasonal Blumea balsamifera leaf volatility
The difference of ingredient, quantitative approach used are similarly area normalization method (Wang Yuanhui, Wang Hongxin, Tian Hongyun, Ma Chaoyang, Chen Tao, Zou
Pure gift, Wang Xing .HS-SPME and GC-MS combination analysis Various Seasonal Blumea balsamifera leaf fragrance componentFood Science, 2012,33
(14): 166.).
Summer millet etc. has studied Blumea balsamifera volatile oil and borneol in different blade profiles and different parts using gas chromatography
Distribution.Be in text first pass through ethyl acetate extract Blumea balsamifera in borneol after, then be measured (Xia Jizi, Chen Gui, An Jun,
Distribution [J] of Zhao Zhi Blumea balsamifera volatile oil and L-Borneol in different blade profiles and different partsChinese patent drug, 2014,36 (8):
1719-1721.).
Wang Yuanhui compares the effect that six kinds of preprocess methods extract borneol in Blumea balsamifera leaf, isoborneol, camphor.It is used
Method is that (Wang Yuanhui, Zhao Dandan, Wang Hongxin, Zou Chunli .GC measure Blumea balsamifera to gas chromatography-mass spectrography combined standard curve method
L-Borneol in leaf, isoborneol, camphor different pretreatments method compare [J]Modern food science and technology, 2014,30 (6): 250-
256.).Six kinds of preprocess methods are respectively as follows: steam distillation, solvent extraction method, simultaneously distillation and extraction method, Microwave-assisted Extraction
It follows the example of, ultrasound assisted extraction method and ultrasound-microwave cooperating extraction method, all methods use solvent extraction step.
The premise of area normalization method is that all components have response in a detector in sample, and assume all chemical combination
The quantitative correction factor of object is a kind of relative amount measuring method in this way.We usually need in actual experiment
It is to be understood that the absolute content of test substance, at this time just needs the methods of calibration curve method or standard addition method.
Traditional extracting process usually requires a large amount of solvents, and extraction efficiency is low, complex for operation step, and extraction time is long.And
Since sample exposure duration is long during the extraction process, some effumability component damages are larger, result in sample message to have in this way
A degree of distortion.In view of the above problems, be badly in need of establishing it is simpler quickly, selectivity is high, use scope is extensive, price is low
Honest and clean, environmental-friendly sample-pretreating method, for the volatile component in quantitative analysis Chinese herbal medicine.
Automatic headspace technique is to analyze a kind of new method of volatile materials in sample substrate, and automatic headspace technique has pair
Sample requirements are small, sample without processing or simple process, do not use solvent, it is environmentally friendly the advantages that.But head space
Report of the technology for quantitative analysis is less.
Through literature survey, at present there has been no by automatic HS GC-mass spectrography, measured using calibration curve method
Borneol in Blumea balsamifera is reported containing quantifier elimination.The present invention is based on automatic HS GC-mass spectrographies, using standard curve
Standard measure measures the absolute content of most important ingredient borneol in Blumea balsamifera, and analysis method quickly, simply, accurately, can be used for Ai Na
The control of the quality of incense drug material or its extract.
Summary of the invention
It is an object of the invention to overcome the shortcomings of the prior art, a kind of simple, quick, accurate, environment friend is provided
The method of borneol absolute content in good measurement Blumea balsamifera.
It is molten to be made into series standard with borneol standard items for the method for borneol absolute content in measurement Blumea balsamifera provided by the invention
Liquid establishes standard curve by automatic HS GC-mass spectrography；The borneol content in Blumea balsamifera leaf powder is measured, from mark
Directrix curve directly checks in the absolute content of borneol in Blumea balsamifera, the specific steps are as follows:
(1) preparation of borneol Standard Stock solutions: precise 150-300 mg borneol is transferred in 25-50 mL volumetric flask,
With ethyl acetate dissolution and constant volume, borneol Standard Stock solutions are obtained；
(2) preparation of borneol series standard solution: 0.1,0.5,1,2,3 mL borneol Standard Stock solutions to 5 mL are pipetted respectively
In volumetric flask, with ethyl acetate constant volume, borneol series standard solution is obtained；
(3) foundation of borneol standard curve: pipetting the borneol series standard solution of each concentration of 20-50 μ L into ml headspace bottle, rotation
Ml headspace bottle waits certain time, so that a large amount of ethyl acetate volatilizations, by automatic HS GC-Mass Spectrometry by choosing
Fixed condition is analyzed；It is mapped with quality of the peak area of borneol to borneol contained in standard solution；Using least square method pair
Data carry out linear fit, obtain the standard curve of borneol；
Regression equation: y=1061855899x+15766221；
Wherein x is borneol quality (mg), and y is the peak area of borneol in chromatogram；
Related coefficient square: R2=0.9920；The range of linearity: 0.002-0.07 mg；Standard curve is shown in Fig. 1；
(4) Blumea balsamifera leaf 2.0-10.0 g is taken, after crushing by pulverizer, samples 40-100 mg immediately in ml headspace bottle, it is close
Envelope presses selected condition analysis by automatic HS GC-Mass Spectrometry, the peak area of borneol is obtained, from standard curve
The content of borneol is read, the absolute content to get borneol in Blumea balsamifera is calculated.
In the present invention, the optimum condition of the automatic HS GC-Mass Spectrometry is as follows:
(1) automatic head space condition: 80-110 DEG C of equilibrium temperature, 90-120 DEG C of loop temperature, 100-130 DEG C of transmission line temperature is put down
Weigh time 10-30 min, and carrier gas is high pure nitrogen or high-purity helium, sample strain 10-20 psi, sample injection time 0.5-2 min；
(2) GC conditions: carrier gas be high pure nitrogen or high-purity helium, flow velocity be 0.5-1.2 mL/min, shunt or regardless of
Sample is flowed into, HP-5 MS quartz capillary column or similar chromatographic column are analyzed using temperature programming；
(3) Mass Spectrometry Conditions: ion source: EI, electron energy: 65-75 eV, electron multiplier voltage: 910 V-930 V, ion source
Temperature: 210 DEG C -240, quadrupole rod temperature: 145 DEG C -160 DEG C, scanning mode: full scan；Mass scan range: 35 ~ 500
m/z；
(4) confirmation of borneol and peak area: 11 standard mass spectrum picture library of NIST is retrieved by chem workstation, confirms the color of borneol
Spectral peak, this is qualitative analysis；By chem workstation data processing system, borneol chromatographic peak is integrated, both obtains borneol peak
Area.
In the present invention, described program heating process are as follows: 50-60 DEG C of initial temperature, keep 1-2min, with 10-12 DEG C/
Min is warming up to 150-160 DEG C, keeps 1-2 min, then be warming up to 210-230 DEG C of holding 1-2 min with 10-12 DEG C/min.
Research and further explanation to said determination condition:
1. reperformance test:
Take 30 μ L or so standard solution in ml headspace bottle, headspace sampling and the peak area for recording borneol.6 parts are measured in parallel, meter
Calculate borneol absolute content relative standard deviation (RSD) be 2.6%.
2. the measurement of the rate of recovery
The preparation of matrix blank sample: the appropriate Blumea balsamifera leaf of crushing is immersed in methanol solution 6-10 hours, is then filtered
Methanol solution is removed, residue continues to be immersed in the mixed solution of acetoneand ethyl acetate 2-4 hours, then on Rotary Evaporators
It removes solvent and obtains blank sample.
50mg blank sample is weighed into 20mL ml headspace bottle, a certain amount of standard solution is then added, carries out the rate of recovery
Experiment, 3 levels contain 0.024 mg of borneol, 0.036 mg, 0.048mg respectively, and each 3 repetitions of horizontal progress are tested, obtained
Average recovery rate be followed successively by 93.3%, 97.7%, 92.6%.
First passage of the present invention establishes standard curve, using automatic HS GC-Mass Spectrometry in Blumea balsamifera
Borneol absolute content is measured, and compensating for previous area normalization method can only obtain the shortcoming of borneol relative amount, energy
The content of borneol in more actual response Blumea balsamifera sample.Meanwhile this method is small to sample requirements, in the measurement of Blumea balsamifera sample not
Using solvent, have many advantages, such as environmentally friendly.
With the method for the present invention (automatic HS GC-mass spectrography) and traditional steam distillation-gas-chromatography-hydrogen fire
Flame ionization detector method carries out ten assays to the borneol in same a collection of Blumea balsamifera.It is examined and t check table by F
It is bright:, it can be said that automatic HS GC-mass spectrography and traditional steam distillation-gas-chromatography-hydrogen fire when 98% confidence level
Flame ionization detector method detection borneol absolute content value is not significantly different.Illustrate this method can be used for Blumea balsamifera medicinal material or its
The quality of extract controls.
Detailed description of the invention
Fig. 1 is automatic HS GC-mass spectrometric determination borneol content standard curve.
Fig. 2 is the standard song that traditional steam distillation-gas-chromatography-flame ionization ditector method measures borneol content
Line.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
The method for quantitative determining borneol in Blumea balsamifera, comprising the following steps:
(1) preparation of borneol Standard Stock solutions: 153 mg borneol of precise is transferred in 25 mL volumetric flasks, with acetic acid second
Ester dissolution and constant volume, obtain borneol Standard Stock solutions；
(2) preparation of borneol series standard solution: 0.1,0.5,1,2,3 mL borneol Standard Stock solutions to 5 mL are pipetted respectively
In volumetric flask, with ethyl acetate constant volume, borneol series standard solution is obtained；
(3) foundation of borneol standard curve: pipetting the borneol series standard solution of 20 each concentration of μ L into ml headspace bottle, rotation top
Empty bottle waits 20 seconds, so that a large amount of ethyl acetate volatilizations, press selected condition by automatic HS GC-Mass Spectrometry
It is analyzed.It is mapped with quality of the peak area of borneol to borneol contained in standard solution.By least square method to data into
Row linear fit obtains the standard curve of borneol；
Regression equation: y=1061855899x+15766221；X is borneol quality (mg), and y is the peak area of borneol in chromatogram；
Related coefficient square: R2=0.9920；The range of linearity: 0.002-0.07 mg；Standard curve is shown in Fig. 1；
(4) 2.0 g of Blumea balsamifera leaf is taken, after crushing by pulverizer, samples 50 mg immediately in 20 mL ml headspace bottles, is sealed, is led to
It crosses automatic HS GC-Mass Spectrometry and presses selected condition analysis, obtain the peak area of borneol, read from standard curve
The content of borneol calculates the absolute content to get borneol in Blumea balsamifera.
The optimum condition of automatic HS GC-Mass Spectrometry is as follows:
(1) automatic head space condition: 20 mL ml headspace bottles, 100 DEG C of equilibrium temperature, 110 DEG C of loop temperature, 120 DEG C of transmission line temperature,
Equilibration time 15 min, carrier gas N2, 15 psi of sample strain, 0.5 min of sample injection time；
(2) GC conditions: carrier gas N2, flow velocity is 1.0 mL/min, split sampling (split ratio 1: 1), HP-5 MS quartz
Capillary column (30 m, 0.25 mm, 0.25 μm)；Temperature programming: 60 DEG C of initial temperature, 1 min is kept, with 12 DEG C/min liter
Temperature keeps 1 min to 160 DEG C, then is warming up to 210 DEG C of 1 min of holding with 12 DEG C/min；
(3) Mass Spectrometry Conditions are as follows, ion source: EI, electron energy: 70 eV, electron multiplier voltage: 918 V, ion source temperature:
230℃；Quadrupole rod temperature: 150 DEG C, scanning mode: full scan, mass scan range: 35 ~ 500 m/z；
(4) confirmation of borneol and peak area: 11 standard mass spectrum picture library of NIST is retrieved by chem workstation, in combination with related
Document is parsed, and confirms the chromatographic peak of borneol, this is qualitative analysis；By chem workstation data processing system, to borneol
Chromatographic peak is integrated, and borneol peak area is both obtained.
Research and detailed description to said determination condition:
1. reperformance test:
Take 30 μ L of standard solution in ml headspace bottle, headspace sampling and the peak area for recording borneol.6 parts are measured in parallel, is calculated
The relative standard deviation (RSD) of borneol absolute content is 2.6%.As a result such as the following table 1.
2. the measurement of the rate of recovery
The preparation of matrix blank sample: the appropriate Blumea balsamifera leaf of crushing is immersed in methanol solution 8 hours, is then filtered to remove
Methanol solution, residue continue to be immersed in the mixed solution of acetoneand ethyl acetate 2 hours, then remove on Rotary Evaporators molten
Agent obtains blank sample.
50mg blank sample is weighed into 20mL ml headspace bottle, a certain amount of standard solution is then added, carries out the rate of recovery
Experiment, 3 levels contain 0.024 mg of borneol, 0.036 mg, 0.048mg respectively, and each 3 repetitions of horizontal progress are tested, obtained
Average recovery rate and relative standard deviation (RSD), be shown in Table 2.
Control experiment, traditional steam distillation-gas-chromatography-flame ionization ditector method operating procedure are as follows:
(1) 103.4 mg hendecanes are weighed to be transferred in 10 mL volumetric flasks, scale is dissolved and be settled to ethyl acetate, is obtained
Concentration is the internal standard standard solution of 10.34 mg/mL；
(2) 63 mg of borneol is accurately weighed, is transferred in 50 mL volumetric flasks, 40 mL or so ethyl acetate, ultrasound 5 minutes is added
To dissolution, ethyl acetate constant volume is used after cooling, obtains the standard reserving solution of borneol.Accurately pipette above-mentioned stock solution 0.1,0.5,1,
2,3,4,5 mL add ethyl acetate to dissolve and are diluted to scale, the interior of 30 uL is then added respectively in 75 mL volumetric flasks
Standard solution is marked, the Working Standard Solution of series of concentrations is obtained.Taking 1 μ L Working Standard Solution respectively, sample introduction is analyzed；
(3) by the retention time at chromatogram confirmation borneol peak, with borneol peak area and internal standard peak area ratio to borneol concentration into
Row linear regression obtains the standard curve regression equation of borneol；Regression equation are as follows:
y=15.6330x-0.0385；Wherein x is borneol concentration (mg/mL), and y is borneol peak area/internal standard peak face in chromatogram
Product；Related coefficient square: R2=0.9995；
(4) it after taking the 20 electronic crushing of g Blumea balsamifera leaf, is transferred in 500 mL round-bottomed flasks.Certain volume is added in bottle
Flask is put into microwave device by water, connects extraction element and condenser pipe, and 10 mL ethyl acetate are put into extractor, setting
Microwave power and time.After the completion of microwave heating refluxing extraction, after waiting extractors natural cooling, by the ethyl acetate in extractor
Solution is released, and is placed in sealed glass jars, dry with anhydrous sodium sulfate, obtains volatile oil ethyl acetate solution.
Traditional steam distillation-gas-chromatography-flame ionization ditector method optimum condition is as follows:
(1) when steam distillation, amount of aqueous solution used is 10 times of material quantity, microwave power 600W, 30 min of Microwave Extraction；
(2) CP-3800 gas chromatograph (fid detector)；Capillary column: CP8510(30 m, 0.25 mm I.D., 0.25 mm
Film)；Carrier gas: nitrogen；Flow velocity: 1mL/min；Split ratio: 20: 1；Temperature program: initial temperature is 60 DEG C, keeps 1 min,
280 DEG C are warming up to 12 DEG C/min, keeps 3 min.
With the method for the present invention (automatic HS GC-mass spectrography) and traditional steam distillation-gas-chromatography-hydrogen fire
Flame ionization detector method carries out ten assays to the borneol in same a collection of Blumea balsamifera.The result ratio of two kinds of measuring methods
Relatively it is shown in Table 3.
The result comparative analysis of two methods is as follows:
Two class problems are commonly encountered in the establishment process of quantitative analysis method, first is that the average value that sample measures and true value are different
It causes；Second be distinct methods measurement average value it is inconsistent.Therefore, it is necessary to the result precision or precision of two kinds of analysis methods
Degree judges (significance test) with the presence or absence of significant difference.The significance test of the common two groups of data of statistical check is suitable
Sequence is that first F is examined, and rear t is examined.
Traditional steam distillation-gas-chromatography-flame ionization ditector method calculates as follows:
=1.3326,n 1=10,S 1=0.1614, S1 2 = 0.0260
Automatic HS GC-mass spectrography calculates as follows:
=1.1993,n 2=10,S 2=0.1119, S2 2 = 0.0125
F is examined:
It looks into F and examines critical table, whenf 1= 9、f 2=9, when confidence level is 95%,F 0.05 =4.03,
BorneolF Meter<F 0.05；
Therefore, F, which is examined, illustrates the variance of borneol in two methods without significant difference, continues to acquire pooled standard deviation as follows:
Total freedom degree
Looking into t examines tables of critical values (unilateral side) to obtain,
The calculated value of borneolt Meter<2.55。
As can be seen from the above results, it can be said that automatic HS GC-mass spectrography and tradition when 98% confidence level
Borneol absolute content value obtained by steam distillation-gas-chromatography-flame ionization ditector method is not significantly different.
The repeated measurement result of table 1.
2. determination of recovery rates result of table and relative standard deviation
Measurement result of 3. two methods of table to borneol content in Blumea balsamifera powder sample
Claims (3)
1. a kind of method of borneol absolute content in measurement Blumea balsamifera, which is characterized in that be made into series standard with borneol standard items
Solution establishes standard curve by automatic HS GC-mass spectrography；The borneol content in Blumea balsamifera leaf powder is measured, from
Standard curve directly checks in the absolute content of borneol in Blumea balsamifera, the specific steps are as follows:
(1) preparation of borneol Standard Stock solutions: 150-300 mg borneol is weighed, is transferred in 25-50 mL volumetric flask, uses second
Acetoacetic ester dissolution and constant volume, obtain borneol Standard Stock solutions；
(2) preparation of borneol series standard solution: 0.1,0.5,1,2,3 mL borneol Standard Stock solutions to 5 mL are pipetted respectively
In volumetric flask, with ethyl acetate constant volume, borneol series standard solution is obtained；
(3) foundation of borneol standard curve: pipetting the borneol series standard solution of each concentration of 20-50 μ L into ml headspace bottle, rotation
Ml headspace bottle waits certain time, so that a large amount of ethyl acetate volatilizations, by automatic HS GC-Mass Spectrometry by choosing
Fixed condition is analyzed；It is mapped with quality of the peak area of borneol to borneol contained in standard solution；Using least square method pair
Data carry out linear fit, obtain the standard curve of borneol；
Regression equation: y=1061855899x+15766221；
Wherein, x is borneol quality (mg), and y is the peak area of borneol in chromatogram；
Related coefficient square: R2=0.9920；The range of linearity: 0.002-0.07 mg；
(4) Blumea balsamifera leaf 2.0-10.0 g is taken, after being crushed by pulverizer, 40-100 mg is sampled in ml headspace bottle, seals, lead to
It crosses automatic HS GC-Mass Spectrometry and presses selected condition analysis, obtain the peak area of borneol, read from standard curve
The content of borneol calculates the absolute content to get borneol in Blumea balsamifera.
2. the method according to claim 1, wherein the item of the automatic HS GC-Mass Spectrometry
Part is as follows:
(1) automatic head space condition: 80-110 DEG C of equilibrium temperature, 90-120 DEG C of loop temperature, 100-130 DEG C of transmission line temperature is put down
Weigh time 10-30 min, and carrier gas is high pure nitrogen or high-purity helium, sample strain 10-20 psi, sample injection time 0.5-2 min；
(2) GC conditions: carrier gas be high pure nitrogen or high-purity helium, flow velocity be 0.5-1.2 mL/min, shunt or regardless of
Sample is flowed into, HP-5 MS quartz capillary column or similar chromatographic column are analyzed using temperature programming；
(3) Mass Spectrometry Conditions: ion source: EI, electron energy: 65-75 eV, electron multiplier voltage: 910 V-930 V, ion source
Temperature: 210 DEG C -240 DEG C, quadrupole rod temperature: 145 DEG C -160 DEG C, scanning mode: full scan；Mass scan range: 35 ~ 500
m/z；
(4) confirmation of borneol and peak area: 11 standard mass spectrum picture library of NIST is retrieved by chem workstation, confirms the color of borneol
Spectral peak, this is qualitative analysis；By chem workstation data processing system, borneol chromatographic peak is integrated, both obtains borneol peak
Area.
3. according to the method described in claim 2, it is characterized in that, the process of described program heating are as follows: initial temperature 50-60
DEG C, 1-2min is kept, 150-160 DEG C is warming up to 10-12 DEG C/min, keeps 1-2 min, then with 10-12 DEG C/min liter
Temperature is to 210-230 DEG C of holding 1-2 min.
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