CN104931605B - Method for detecting quality of pepper powder based on component analysis - Google Patents
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Abstract
The invention discloses a method for detecting the quality of pepper powder based on component analysis. A certain amount of the pepper powder is distilled through water vapor to prepare a pepper extract solution, the obtained pepper extract solution is subjected to component analysis through a gas chromatographic mass spectrometry method, characteristic chemical components including linalool, linalyl acetate, beta-caryophyllene and alpha-caryophyllene in the pepper extract solution are selected as main target components, phenylethyl propionate is selected as an internal standard substance, and linalool, linalyl acetate, beta-caryophyllene and alpha-caryophyllene in the pepper extract solution are quantitatively analyzed with a selected ion gas chromatographic mass spectrometry method to determine the content and range of linalool, linalyl acetate, beta-caryophyllene and alpha-caryophyllene. The method for detecting the quality of the pepper powder based on the component analysis is capable of quickly, simply, flexibly and accurately detecting the quality of the pepper powder and can be widely applied.
Description
Technical field
The invention belongs to flavoring agent technical field of quality detection, is related to a kind of Zanthoxyli Bungeani powder quality testing based on component analyses
Method, specifically refers to using the linalool in gas chromatograph-mass spectrometer (GC-MS) detection Zanthoxyli Bungeani powder, linalyl acetate, second position Dianthus chinensis
The quality determining method of alkene and first position caryophyllene content.
Background technology
In recent years, in China's field of food safety, all kinds of false and personation food event takes place frequently.People's material life water
Benefit is improved on ordinary days, but, on dining table, the color, smell and taste of delicacies are but had a greatly reduced quality, and Pericarpium Zanthoxyli is not numb, and Fructus Capsici is not peppery, and Oleum sesami is not fragrant.As
Food production raw material toppings are adulterated of common occurrence, and the common practices of fraud are that other relatively low things of price are mixed in food
Matter, wherein most are the non-edible material from soybeans being detrimental to health, and consumer is generally difficult to recognize these food.
Pericarpium Zanthoxyli is that the maturation of Rutaceae xanthoxylum, Pericarpium Zanthoxyli or Zanthoxylum schinifolium is dried peel, and in China, most area is equal
There is production.There is warming middle-JIAO to relieve pain, killing parasites for relieving itching, important flavoring agent, spice, with battalion is also used as in addition
Foster function.Zanthoxyli Bungeani powder be with Pericarpium Zanthoxyli as raw material Jing grinds, screens, packing made by single Zanthoxyli Bungeani powder product.With Pericarpium Zanthoxyli as raw material
The Zanthoxyli Bungeani powder of production is a kind of material of spice of high-quality, and many material of spice of production of condiments enterprise application amount it
One, but the examination criteria at present to Zanthoxyli Bungeani powder, and the typically just physics and chemistry for Zanthoxyli Bungeani powder and microorganism make index, simply lean on
Perusal and taste identification can not accurately judge its feedstock property, so that both easily entering in the vacation of Zanthoxyli Bungeani powder processing variety
OK, it is and lucrative.
Gaschromatographic mass spectrometry (GC-MS) method is a kind of quick, simplicity, accurately and efficiently analysis and detection technology, extensively
For the analysis of various natural components in plant, including the Components identification and content detection in the volatile oil in plant.Volatile oil
Also known as quintessence oil, be a class plant source secondary metabolites, be molecular weight in plant body, can steam with vapor, with one
Determine the volatility oily liquid substance of abnormal smells from the patient.
The fragrance component of Pericarpium Zanthoxyli comes from volatile oil contained during which is organized, and in Pericarpium Zanthoxyli, the content of volatile oil is typically 0.7%
~ 0.9%, the Pericarpium Zanthoxyli volatile oil chemical composition of different cultivars and content difference it is larger, even same kind, due to weather, the place of production
Deng impact, the content and proportion of composing of volatile oil be also different.Volatile flavor component is comprised only in the volatile oil of Pericarpium Zanthoxyli, its
Spicy composition does not have volatility.Chen Xiaoquan exists《Plant chemotaxonomy》In mention：In volatile oil, key component is olefines
With b- phellandrenes, limonene, b- pinenes, a- pinenes, b- ocimenes etc., these materials are widely used in spice, food industry and medicine
The important intermediate of thing synthesis；The also oxygenatedchemicalss of hydro carbons, including alcohols such as linalool, terpinol etc., it is similar such as Fructus Piperiss
Ketone, menthone etc., also aldehydes, esters and epoxy compound species etc., these materials are promoting the release of human body hormone, improve first
The aspects such as the infiltration of shape parathyrine play an important role.Yan Jianhui analyzes the chemical composition of volatile oil of Pericarpium Zanthoxyli by GC-MS, finds
In the component identified, 18 kinds of hydrocarbon compound accounts for the 24.68% of tested total amount, wherein Dianthus chinensis alkenes（A- caryophyllene 1.56%,
B- caryophyllene 6.88%）, what in component, content was most is terpin alcohol compound, wherein b- linalools（Linalool）Content
0.96%.Wu Surui extracts the quintessence oil in Pericarpium Zanthoxyli by Simultaneous distillation, and the quintessence oil of extraction is carried out GC-MS analyses, grinds
The fragrance composition and feature of Pericarpium Zanthoxyli are studied carefully, it is found that the contribution of each material is descending in Pericarpium Zanthoxyli fragrance and be arranged as linalool, Chinese juniper
Alkene, b- myrcenes, a- pinenes, limonene, a- ketone, a- alkene, 4- terpineol, b- pinenes, geraniol, a- terpinolene, a-
Terpineol, nerolidol, acetic acid linalool, piperitol, b- ketone.
The extracting method of volatile oil mainly include the conventional steam way of distillation, solvent extraction, supercritical carbon dioxide fluid extraction,
Simultaneous distillation etc., wherein steam distillation are most traditional essential oil extraction methods, with behaviour simplicity, low cost,
The features such as being easily achieved, is relatively adapted to the operation of laboratory sample.
For still lacking the effective Zanthoxyli Bungeani powder quality detection technology of complete set at present, therefore, it is necessary to research and develop a kind of letter
The reliable and stable Zanthoxyli Bungeani powder quality determining method of single rapid, result is filling up the blank of prior art.
The content of the invention
It is an object of the invention to provide a kind of employing GC-MS is to the linalool in Zanthoxyli Bungeani powder, acetic acid Lignum cinnamomi camphorae
Ester, second position caryophyllene and first position caryophyllene content detected, its can more rapidly, it is easy, detect Zanthoxyli Bungeani powder flexibly, exactly
Quality, can be used for Zanthoxyli Bungeani powder enterprise-quality acceptance criteria.
The present invention is by the following technical programs to realize above-mentioned purpose, a kind of Zanthoxyli Bungeani powder quality based on component analyses
Detection method, comprises the following steps：
（1）The preparation of Pericarpium Zanthoxyli extracting solution：Precision weighs Zanthoxyli Bungeani powder sample 10g, is placed in flask, adds 95% second of 50mL
Alcohol, is heated to reflux 3h, after being cooled to room temperature, solution is filtered in brown volumetric flask, with alcohol flushing bottle,suction and filter 3
Secondary, washing liquid is filtered in volumetric flask in the lump, and adds ethanol to scale, is shaken up standby；
（2）The preparation of inner mark solution：Phenylethyl propionate is weighed, the ethanol solution of phenylethyl propionate is prepared, it is molten as internal standard
Liquid, it is standby；
（3）The preparation of standard working solution：Linalool, linalyl acetate, second position caryophyllene and first position caryophyllene are weighed, is used
Simultaneously constant volume, in volumetric flask, as standard reserving solution, standard reserving solution is prepared containing virtue by stepwise dilution for inner mark solution dissolving
The series standard working solution of Camphor tree alcohol, linalyl acetate, second position caryophyllene and first position caryophyllene；
（4）The process of sample：Precision weighs 1.5g steps（1）The Pericarpium Zanthoxyli extracting solution of preparation, adds step（2）What is prepared is interior
Mark solution 5.0mL, stands after fully vibrating, and filters, used as treating test sample；
（5）The measure of sample：
The chromatographic condition of gas chromatography mass spectrometer：Using nonpolar chromatographic column, carrier gas is high-purity helium, and column flow rate is 1mL/
Min constant currents, split ratio 1:1, sample size：1 μ L, injector temperature are 250 DEG C, and temperature programming is 60 DEG C of post initial temperature, is kept
2min, is raised to 150 DEG C with the speed of 3 DEG C/min, keeps 1min, is then raised to 280 DEG C with the speed of 15 DEG C/min, keeps
4min；
The Mass Spectrometry Conditions of gas chromatography mass spectrometer：Interface temperature is 280 DEG C, and ion source temperature is 250 DEG C, level Four bar temperature
For 150 DEG C, ionizing energy is 70eV, solvent time delay 3min, and full scan mass ranges are 50 ~ 450amu, Salbutamol Selected Ion Monitoring mould
Formula；
Take 1 μ L to treat test sample, standard substance and treat test sample addition standard substance, be injected separately into gas chromatography mass spectrometer, third
Sour phenethyl ester, linalool, linalyl acetate, second position caryophyllene and first position caryophyllene are respectively with m/z as 105,178；71,93；80,
93,121；93,133；93,121 ions are quantitative, draw standard curve, sample and standard curve fit using internal standard method, draw examination
The content of linalool, linalyl acetate, second position caryophyllene and first position caryophyllene in sample.
Further, the step（2）In phenylethyl propionate concentration be 100 μ g/mL.
Further, the step（3）In series standard working solution concentration be respectively 10 μ g/mL, 25 μ g/mL,
50μg/mL、100μg/mL、150μg/mL、250μg/mL。
Further, the step（4）Used in 0.45 μm organic faciess filter membrane filtration.
Further, the step（5）In nonpolar chromatographic column be HP-5MS.
The Zanthoxyli Bungeani powder sample of 10 batches is tested in the Zanthoxyli Bungeani powder quality determining method of component analyses using the present invention,
Determine linalool in Zanthoxyli Bungeani powder, linalyl acetate, second position caryophyllene and first position caryophyllene content range be respectively 30.81 ~
37.65mg/g, 13.76 ~ 16.82mg/g, 1.58 ~ 1.92mg/g, 2.07 ~ 2.53mg/g.In the inventive method, linalool is reclaimed
Rate is 102.41% ~ 103.71%, and meansigma methodss are 103.07%；The linalyl acetate response rate is 97.48 ~ 102.79%, and meansigma methodss are
99.46%；The second position caryophyllene response rate is 86.71% ~ 91.92%, and meansigma methodss are 89.26%；The first position caryophyllene response rate is
82.50% ~ 91.05%, meansigma methodss are 85.72%.
Therefore, advantage of the invention is that：
The present invention is that one kind adopts GC-MS to Pericarpium Zanthoxyli based on the Zanthoxyli Bungeani powder quality determining method of component analyses
The method that linalool, linalyl acetate and second position caryophyllene, first position caryophyllene mark in powder carries out detection by quantitative, with preferable
Method repeatability, accuracy are high, can meet the needs to Zanthoxyli Bungeani powder content detection in real work, while the inventive method operation
It is simple rapid, it is as a result reliable and stable, it is adaptable in the quality control efforts of Zanthoxyli Bungeani powder, test in particular for Zanthoxyli Bungeani powder enterprise-quality
Receipts standard.
Description of the drawings
The standard substance ion flow graph that Fig. 1 GC-MS SIM methods are obtained, wherein a- linalools, b- linalyl acetates, c-
Phenylethyl propionate, d- second position caryophyllene, e- first position caryophyllene.
The ion flow graph of the Pericarpium Zanthoxyli extracting solution that Fig. 2 GC-MS SIM methods are obtained, wherein a- linalools, b- acetic acid Lignum cinnamomi camphorae
Ester, c- phenylethyl propionates, d- second position caryophyllene, e- first position caryophyllene.
The Pericarpium Zanthoxyli extracting solution and Pericarpium Zanthoxyli extracting solution that Fig. 3 GC-MS SIM methods are obtained adds the ion stream after standard substance
Figure, wherein a- linalools, b- linalyl acetates, c- phenylethyl propionates, d- second position caryophyllene, e- first position caryophyllene.
The standard working curve of Fig. 4 linalools.
The standard working curve of Fig. 5 linalyl acetates.
The standard working curve of Fig. 6 second position caryophyllene.
The standard working curve of Fig. 7 first position caryophyllene.
Specific implementation method
The present invention is further described below by way of specific embodiment, but the present invention is not limited only to following examples.
In the scope of the present invention or in without departing from present disclosure, spirit and scope, to Zanthoxyli Bungeani powder quality of the present invention
Detection method is carried out being suitably modified, replaces effect identical component, it will become apparent to those skilled in the art that it
Be considered as being included within the scope of the present invention.
Embodiment 1, the Zanthoxyli Bungeani powder quality determining method based on component analyses
1st, experiment reagent and instrument：
1.1 reagent：Ethanol（Analysis is pure）, phenylethyl propionate, linalool, linalyl acetate, second position caryophyllene, first position Dianthus chinensis
Alkene, pure water.
1.2 instrument：GC7890A-5973C gas chromatography mass spectrometers（Aglient companies of the U.S.）, electronic balance, backflow dress
Put.
, experimental technique：
2.1 experiment condition：
2.1.1 the chromatographic condition of gas chromatography mass spectrometer：Nonpolar chromatographic column：HP-5MS(30 m x 250 μm x
0.25 μm)；Carrier gas：High-purity helium；Column flow rate：1mL/min constant currents；Split ratio：1:1, injector temperature：250℃；Sample size：
1μL；Temperature programming：60 DEG C of post initial temperature, keep 2min, be raised to 150 DEG C with the speed of 3 DEG C/min, keep 1min, then with
The speed of 15 DEG C/min is raised to 280 DEG C, keeps 4min.
2.1.2 the Mass Spectrometry Conditions of gas chromatography mass spectrometer：Interface temperature：280℃；Ion source temperature：250℃；Level Four bar
Temperature：150℃；Ionizing energy：70eV；Solvent time delay：3min；Full scan mass ranges：50~450amu；Salbutamol Selected Ion Monitoring
Pattern.
2.2 experimentation：
（1）The preparation of Pericarpium Zanthoxyli extracting solution：Precision weighs Zanthoxyli Bungeani powder sample 10g, is placed in 250mL flasks, adds 50mL
95% ethanol, loads onto reflux condensing tube, is heated to boiling, maintains the reflux for 3h, after being cooled to room temperature, solution is filtered and is held into 100mL browns
In measuring bottle, with alcohol flushing bottle,suction and filter 3 times, washing liquid is filtered in volumetric flask in the lump, and plus ethanol to scale, shake up standby
With；
（2）The preparation of inner mark solution：Compound concentration is the ethanol solution of the phenylethyl propionate of 100 μ g/mL, molten as internal standard
Liquid；
（3）The preparation of standard working solution：Linalool, linalyl acetate, second position caryophyllene and first position caryophyllene are weighed, is used
Simultaneously constant volume, in volumetric flask, as standard reserving solution, standard reserving solution is prepared containing virtue by stepwise dilution for inner mark solution dissolving
Camphor tree alcohol, linalyl acetate, second position caryophyllene and first position caryophyllene be respectively 10 μ g/mL, 25 μ g/mL, 50 μ g/mL, 100 μ g/mL,
The standard working solution of 150 μ g/mL, 250 μ g/mL；
（4）The process of sample：Precision weighs 1.5g steps（1）The Pericarpium Zanthoxyli extracting solution of preparation, adds step（2）Third for preparing
Sour phenethyl ester inner mark solution 5.0mL, stands after fully vibrating, and filters membrane filtration with 0.45 μm of organic faciess, used as treating test sample；
（5）The measure of sample：Take 1 μ L to treat test sample, standard substance and treat test sample addition standard substance, be injected separately into gas phase
Chromatographic mass spectrometry instrument, phenylethyl propionate, linalool, linalyl acetate, second position caryophyllene and first position caryophyllene respectively with m/z as 105,
178；71,93；80,93,121；93,133；93,121 ions are quantitative, measurement result as shown in Figure 1, Figure 2 and Figure 3；Using internal standard
Method draws the standard curve of linalool, linalyl acetate, second position caryophyllene and first position caryophyllene respectively such as Fig. 4, Fig. 5, Fig. 6 and Tu
Shown in 7, linalool y=525.08x, correlation coefficient：0.9986；Linalyl acetate y=142.23x, correlation coefficient：0.9995；Second
Position caryophyllene y=256.21x, correlation coefficient：0.9997；First position caryophyllene y=806.26, correlation coefficient：0.9996.Sample and mark
Directrix curve is fitted, and show that the content of linalool, linalyl acetate, second position caryophyllene and first position caryophyllene in sample is respectively
34.23 μ g/g, 13.96 μ g/g, 1.70 μ g/g, 2.21 μ g/g.
Embodiment 2, the Zanthoxyli Bungeani powder quality determining method based on component analyses
The present embodiment to number the Zanthoxyli Bungeani powder sample as HD11008 as detection object, with the operation side of the embodiment of the present invention 1
Method is tested to the Zanthoxyli Bungeani powder sample of 10 batches, each sample parallel assay twice, respectively to the linalool in Zanthoxyli Bungeani powder, second
Sour Lignum cinnamomi camphorae ester, second position caryophyllene and first position caryophyllene are carried out quantitatively, and content range is testing result（Meansigma methodss）± 10%, knot
Fruit see the table below 1.
Linalool, linalyl acetate, second position caryophyllene and first position caryophyllene content in 1 Zanthoxyli Bungeani powder of table
From upper table 1, gas chromatogram matter is carried out to the Pericarpium Zanthoxyli extracting solution for obtaining by controllable sample pre-treatments step
Spectrometry quantitative analyses, determine the content range of linalool, linalyl acetate, second position caryophyllene and first position caryophyllene in Zanthoxyli Bungeani powder
Respectively 30.81 ~ 37.65mg/g, 13.76 ~ 16.82mg/g, 1.58 ~ 1.92mg/g, 2.07 ~ 2.53mg/g.The present invention is based on
The Zanthoxyli Bungeani powder quality determining method of component analyses is simple to operate rapid, as a result reliable and stable, it is adaptable to the quality control of Zanthoxyli Bungeani powder
In work.
The same Zanthoxyli Bungeani powder sample with numbering as HD11008 adds linalool, linalyl acetate, second position as detection object
Caryophyllene and first position caryophyllene standard concentration are respectively 50 μ g/mg, and 25 μ g/mg, 10 μ g/mg, 5 μ g/mg carry out recovery of standard addition
Test, parallel assay 6 times, as a result such as table 2 below.
The response rate of 2 the inventive method of table
From upper table 2, the linalool response rate is 102.41% ~ 103.71%, and meansigma methodss are 103.07%；Linalyl acetate
The response rate is 97.48 ~ 102.79%, and meansigma methodss are 99.46%；The second position caryophyllene response rate is 86.71% ~ 91.92%, and meansigma methodss are
89.26%；The first position caryophyllene response rate is 82.50% ~ 91.05%, and meansigma methodss are 85.72%.This experiment shows to use gas chromatogram
Mass spectrography carries out the side of detection by quantitative to the linalool in Zanthoxyli Bungeani powder, linalyl acetate, second position caryophyllene and first position caryophyllene mark
Method has a preferable method repeatability, and accuracy is high, meets the needs to Zanthoxyli Bungeani powder content detection in real work.
The above is only the preferred embodiment of the present invention, it is noted that it is right that above-mentioned preferred implementation is not construed as
The restriction of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch also to should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of Zanthoxyli Bungeani powder quality determining method based on component analyses, it is characterised in that comprise the following steps：
（1）The preparation of Pericarpium Zanthoxyli extracting solution：Precision weighs Zanthoxyli Bungeani powder sample 10g, is placed in flask, adds 95% ethanol of 50mL, plus
Hot reflux 3h, after being cooled to room temperature, solution is filtered in brown volumetric flask, with alcohol flushing bottle,suction and filter 3 times, washing liquid
Filter in volumetric flask in the lump, and add ethanol to scale, shake up standby；
（2）The preparation of inner mark solution：Phenylethyl propionate is weighed, the ethanol solution of phenylethyl propionate is prepared, it is as inner mark solution, standby
With；
（3）The preparation of standard working solution：Linalool, linalyl acetate, second position caryophyllene and first position caryophyllene are weighed, internal standard is used
Solution dissolving constant volume is in volumetric flask, as standard reserving solution, standard reserving solution is prepared by stepwise dilution contain linalool,
The series standard working solution of linalyl acetate, second position caryophyllene and first position caryophyllene；
（4）The process of sample：Precision weighs 1.5g steps（1）The Pericarpium Zanthoxyli extracting solution of preparation, adds step（2）The internal standard of preparation is molten
Liquid 5.0mL, stands after fully vibrating, and filters, used as treating test sample；
（5）The measure of sample：
The chromatographic condition of gas chromatography mass spectrometer：Using nonpolar chromatographic column, carrier gas is high-purity helium, and column flow rate is 1mL/min
Constant current, split ratio 1:1, sample size：1 μ L, injector temperature are 250 DEG C, and temperature programming is 60 DEG C of post initial temperature, is kept
2min, is raised to 150 DEG C with the speed of 3 DEG C/min, keeps 1min, is then raised to 280 DEG C with the speed of 15 DEG C/min, keeps
4min；
The Mass Spectrometry Conditions of gas chromatography mass spectrometer：Interface temperature is 280 DEG C, and ion source temperature is 250 DEG C, and level Four bar temperature is
150 DEG C, ionizing energy is 70eV, solvent time delay 3min, and full scan mass ranges are 50 ~ 450amu, Salbutamol Selected Ion Monitoring pattern；
Take 1 μ L to treat test sample, standard substance and treat test sample addition standard substance, be injected separately into gas chromatography mass spectrometer, propanoic acid benzene
Ethyl ester, linalool, linalyl acetate, second position caryophyllene and first position caryophyllene are respectively with m/z as 105,178；71,93；80,93,
121；93,133；93,121 ions are quantitative, draw standard curve, sample and standard curve fit using internal standard method, draw sample
The content of middle linalool, linalyl acetate, second position caryophyllene and first position caryophyllene.
2. the Zanthoxyli Bungeani powder quality determining method based on component analyses as claimed in claim 1, it is characterised in that the step
（2）In phenylethyl propionate concentration be 100 μ g/mL.
3. the Zanthoxyli Bungeani powder quality determining method based on component analyses as claimed in claim 1, it is characterised in that the step
（3）In series standard working solution concentration be respectively 10 μ g/mL, 25 μ g/mL, 50 μ g/mL, 100 μ g/mL, 150 μ g/mL,
250μg/mL。
4. the Zanthoxyli Bungeani powder quality determining method based on component analyses as claimed in claim 1, it is characterised in that the step
（4）Used in 0.45 μm organic faciess filter membrane filtration.
5. the Zanthoxyli Bungeani powder quality determining method based on component analyses as claimed in claim 1, it is characterised in that the step
（5）In nonpolar chromatographic column be HP-5MS.
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| CN107045028A (en) * | 2017-03-27 | 2017-08-15 | 许昌学院 | A kind of place of production mixing Chinese prickly ash content authentication method of Zhengzhou Hanyuan two |
| CN107048324A (en) * | 2017-05-10 | 2017-08-18 | 上海应用技术大学 | A kind of Chinese prickly ash essence and preparation method thereof |
| CN108760984B (en) * | 2018-05-08 | 2019-06-07 | 河南省林业科学研究院 | It can be used for the Chinese prickly ash quality detecting method of Chinese prickly ash Adulteration identification |
| CN109613161A (en) * | 2018-12-27 | 2019-04-12 | 苏州科铭生物技术有限公司 | A kind of β based on headspace gas chromatography-carypohyllene content assaying method |
| CN111257467B (en) * | 2020-02-28 | 2022-07-12 | 云南卓一食品有限公司 | Method for detecting linalool hand isomer and application thereof |
| CN116338020A (en) * | 2022-10-26 | 2023-06-27 | 西北农林科技大学 | Method for detecting volatile terpenoid in pepper fruits and application thereof |
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