CN109444284A - Method that is a kind of while measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product - Google Patents
Method that is a kind of while measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product Download PDFInfo
- Publication number
- CN109444284A CN109444284A CN201811533692.0A CN201811533692A CN109444284A CN 109444284 A CN109444284 A CN 109444284A CN 201811533692 A CN201811533692 A CN 201811533692A CN 109444284 A CN109444284 A CN 109444284A
- Authority
- CN
- China
- Prior art keywords
- sanshool
- green pepper
- oil
- chinese prickly
- prickly ash
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
- Seasonings (AREA)
Abstract
The present invention provides a kind of methods for measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product simultaneously, it is characterised in that: it is detected using high performance liquid chromatography, and operating procedure is as follows: 1) preparing reference substance solution;2) test solution is prepared;3) reference substance solution is drawn respectively and test solution injects liquid chromatograph.The method of flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product is measured while of the invention, it can be used for measuring chemical component hydroxyl-alpha-sanshool, the hydroxy-beta-sanshool, hydroxyl-γ-sanshool of " fiber crops " in flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product, and chemical component limonene, the linalool of " perfume " simultaneously.Method is easy, result is reliable, is of great significance, has a good application prospect to the quality control of Chinese prickly ash and/or rattan green pepper and its Related product and scientific evaluation.
Description
Technical field
Present invention relates particularly to a kind of methods for measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product simultaneously.
Background technique
Commercially available Chinese prickly ash commodity mainly include Chinese prickly ash (ZanthoxylumbungeanumMaxim.) and rattan green pepper
Two kinds of (Zanthoxylumarmatum DC.) is a kind of product of the dual-purpose of drug and food of characteristic.As edible product, " fiber crops, perfume " is
Its main flavor characteristic is with spicy fresh perfume for flavouring indispensable in the Sichuan cuisine of characteristic;As medicinal product, embody
The chemical component of " fiber crops, fragrant " is also its main active constituent, research find the active constituent in Chinese prickly ash commodity to digestive system,
In terms of nervous system, the circulatory system and anti-inflammatory, analgesia, antitumor, anti-oxidant, antibacterial desinsection there is stronger pharmacological activity to make
With.Currently, Chinese prickly ash (rattan green pepper) master is used in the form of two kinds of Seasoning Ingredients and processed goods (Zanthoxylum essential oil/Tengjiao oil) as food, flower
Green pepper oil (Tengjiao oil) is directly to impregnate Chinese prickly ash (rattan green pepper) or application organic solvent extraction, SCF-CO 2 etc. side with edible oil
Chinese prickly ash made from method (rattan green pepper) essential oil mixes the made flavored oils with spicy hot taste with appropriate amount of edible oil.
Fragrance matter in Chinese prickly ash commodity is mainly the volatility such as volatile oil, including alkenes, alcohols, ketone, aldehydes, esters
Ingredient, volatile oil is higher with limonene, linalool content in Chinese prickly ash, wherein limonene content highest, and rattan green pepper is with linalool, lemon
Alkene content is higher, wherein linalool content highest;Spicy components are mainly using sanshool as the unsaturated fat of the chain of representative
Sour amide substance mainly includes hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool etc., Chinese prickly ash and rattan green pepper
In all with hydroxyl-alpha-Chinese pepper cellulose content highest.Currently, in the quality assessment standard of Chinese prickly ash (rattan green pepper) and Zanthoxylum essential oil (Tengjiao oil)
In, mostly using sensory evaluation as main method, and the bound requirements of each standard have difference, this make to Chinese prickly ash (rattan green pepper) and
The spicy hot taste of Zanthoxylum essential oil (Tengjiao oil) determines that shortage is scientific, does not have accuracy and objectivity, it is difficult to realize standardization and determine
Quantization.Although part research has carried out quantitative analysis to spicy components or fragrance matter, the flavor substance of Chinese prickly ash includes fiber crops
Taste substance and fragrance matter.Single measurement fragrance matter content or the content of spicy components are as Chinese prickly ash or Zanthoxylum essential oil
Quality assessment standard does not have representativeness, cannot really reflect the inherent product of Chinese prickly ash (rattan green pepper) and Zanthoxylum essential oil (Tengjiao oil) comprehensively
Matter.
Spicy components detection method of content mainly has ultraviolet spectrophotometry and high performance liquid chromatography (HPLC) etc. at present,
The case where wherein what spectrophotometry measured is the content of total spicy components, cannot reflect each spicy component.HPLC method has easy
Operation, the features such as high sensitivity and stability are good, it has also become the main method of analysis measurement spicy components.However in Zanthoxylum essential oil
In the measurement of (Tengjiao oil) spicy components, frequently with the spicy components in methanol extraction Zanthoxylum essential oil (Tengjiao oil), to being formed after extraction
Immiscible two liquid carry out liquid separation methanol solution taken to be analyzed, method easily causes Zanthoxylum essential oil (Tengjiao oil) spicy components
Not exclusively, quantitative analysis is inaccurate for extraction.Currently, fragrance matter assay frequently with gas chromatography measurement limonene and
Linalool content, and gas chromatography operation is more complex, danger coefficient is higher, and popularization is more difficult, using high performance liquid chromatography
Measurement Chinese prickly ash (rattan green pepper) and Zanthoxylum essential oil (Tengjiao oil) fragrance matter are seldom related to, and do not measure spicy components and flavor more simultaneously
The report of matter.Therefore, a kind of easy, accurate numb taste object analyzed in measurement Chinese prickly ash (rattan green pepper) and Zanthoxylum essential oil (Tengjiao oil) is established
Matter and fragrance matter are the method for corporate target, and the objective quality standard of science is established to it, to Chinese prickly ash (rattan green pepper) and its
The quality of Related product controls and scientific evaluation is of great significance.
Summary of the invention
To solve the above problems, measuring flavor in Chinese prickly ash and/or rattan green pepper and its oil product simultaneously the present invention provides a kind of
The method of substance, it is characterised in that: it is detected using high performance liquid chromatography, and operating procedure is as follows:
1) hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool, lemon the preparation of reference substance solution: are taken
Alkene, linalool reference substance, add isopropanol to dissolve, freezen protective, as reference substance solution;
2) preparation of test solution:
A Chinese prickly ash or rattan green pepper test sample: taking test sample to crush, and sieving adds edible oil extract, filters, and extracting solution adds isopropanol
Dissolution, filtering, takes filtrate as test solution;
B Zanthoxylum essential oil or Tengjiao oil test sample: taking test sample, isopropanol added to dissolve, and filtering takes filtrate molten as test sample
Liquid;
3) reference substance solution being drawn respectively and test solution injecting liquid chromatograph, chromatographic condition is as follows:
Chromatographic column: using octadecylsilane chemically bonded silica as filler;Mobile phase: being stream with water using acetonitrile as mobile phase A
Dynamic phase B gradient elution;Gradient elution program is as follows:
Further, the step 1) reference substance solution hydroxyl-α-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-mountain
Green pepper element, limonene, linalool concentration are respectively 800ug/mL, 90ug/mL, 80ug/mL, 2000ug/mL, 1000ug/mL.
Further, the step 1) cryogenic temperature is -20 DEG C.
Further, the sieve of sieving described in step a is No. three sieves.
Further, the mass volume ratio of Chinese prickly ash or rattan green pepper sample to be tested described in step a and edible oil is 10g:60mL, institute
Stating edible oil is corn oil.
Further, extracting at constant temperature, extraction time 150min are extracted as described in step a, extraction temperature is 80 DEG C.
Further, the volume ratio of extracting solution and isopropanol described in step a is 1:50;And/or Zanthoxylum essential oil described in step b
Or the volume ratio of Tengjiao oil sample to be tested and isopropanol is 1:50.
Further, the reference substance solution and test solution amount that liquid chromatograph is injected separately into described in step 3) are 5 μ
l。
Further, step 3) the octadecylsilane chemically bonded silica chromatographic column are as follows: Shiseido CAPCELL PAK C18
Column, 250mm × 4.6mm, 5 μm, MGII.
Further, flow velocity is 1.00mL/min in the step 3) chromatographic condition;Column temperature is 30 DEG C.
Further, step 3) the chromatographic condition medium wavelength is respectively 200nm, 270nm.
The method that flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product is measured while of the invention, can be used for surveying simultaneously
Determine the chemical component hydroxyl-alpha-sanshool, hydroxy-beta-Chinese pepper of " fiber crops " in flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product
Element, hydroxyl-γ-sanshool, and chemical component limonene, the linalool of " perfume ".Method is easy, result is reliable, to Chinese prickly ash (rattan
Green pepper) and its Related product quality control and scientific evaluation be of great significance, have a good application prospect.
Obviously, above content according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific embodiment of form by the following examples remakes further specifically above content of the invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on above content of the present invention
The technology realized all belongs to the scope of the present invention.
Detailed description of the invention
Fig. 1 hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool are in 190-400nm wave-length coverage
Abosrption spectrogram.
The abosrption spectrogram of Fig. 2 linalool, limonene in 190-400nm wave-length coverage.
1 gradient elution liquid phase chromatogram of Fig. 3 scheme (A: wavelength 270nm, B: wavelength 200nm).
2 gradient elution liquid phase chromatogram of Fig. 4 scheme (A: wavelength 270nm, B: wavelength 200nm).
3 gradient elution liquid phase chromatogram of Fig. 5 scheme (A: wavelength 270nm, B: wavelength 200nm).
Fig. 6 Chinese prickly ash (oil) high-efficient liquid phase chromatogram (A: wavelength 270nm, B: wavelength 200nm).
Fig. 7 rattan green pepper (oil) high-efficient liquid phase chromatogram (A: wavelength 270nm, B: wavelength 200nm).
Specific embodiment
1, material, reagent and instrument
1.1 laboratory apparatus
Shimadzu LC-2010A high performance liquid chromatograph, SIL-20A autosampler, SPD-20A detector, CTO-20A column
Incubator, LC solution chromatographic work station software, Japanese Shimadzu Corporation;TU-1901 dual-beam ultraviolet-uisible spectrophotometer
(Beijing Puxi General Instrument Co., Ltd);DZKW thermostat water bath (Beijing Zhong Xing great achievement Co., Ltd).
SartoriusBP211D electronic balance (Sartorius AG);HX-200 type high speed medicinal herb grinder (Zhejiang Province Yongkang City
Small stream bank hardware medical instrument factory);The excellent general serial Superpure water machine of UPT-11-10T.
1.2 materials and reagent
Spicy components reference substance: numb-taste components reference substance: hydroxyl-alpha-sanshool (self-control, purity 98.35%);Hydroxyl
Base-β-sanshool (self-control, apply for into national standard, purity 98.27%);Hydroxyl-γ-sanshool (self-control, purity
98.54%).Fragrance matter reference substance: (purity is for limonene (purity 96%, lot number 100472-201503) and linalool
97.8%, lot number 111503-201603) reference substance is purchased from National Institute for Food and Drugs Control.Isopropanol (analysis is pure, at
City Cologne Chemical Company), methanol (chromatographically pure, sigma company, the U.S.) acetonitrile (chromatographically pure, sigma company, the U.S.),
Water is that ultrapure water is made in laboratory by oneself.
Chinese prickly ash sample is collected in Hanyuan County, sichuan Province, Gansu Wudu, Hancheng Region, Shaanxi;Rattan green pepper sample is collected in sichuan shantai, Sichuan
Jinyang, Sichuan Hongya;Zanthoxylum essential oil and Tengjiao oil sample are bought in supermarket, including bull market slope Zanthoxylum essential oil, nine bucket bowl Zanthoxylum essential oils, Yongfeng
And Zanthoxylum essential oil;Ten thousand not Tengjiao oil, pockmarks Tengjiao oil, bull market slope Tengjiao oils.
The measurement of 1 Chinese prickly ash of embodiment (rattan green pepper) flavor substance
1) preparation of reference substance solution: precision weighs hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-mountain respectively
Green pepper element, linalool, limonene reference substance are dissolved with isopropanol respectively in 5 volumetric flasks and are settled to scale and obtain concentration and be
The reference substance stock solution of 8mg/mL, 0.9mg/mL, 0.8mg/mL, 20mg/mL, 10mg/mL, then 1mL mother liquor is respectively taken to hold in 10mL
The mixing reference substance of 800 μ g/mL, 90 μ g/mL, 80 μ g/mL, 2000 μ g/mL, 1000 μ g/mL are made of isopropanol constant volume for measuring bottle
Mother liquor stores it under the conditions of -20 DEG C for liquid phase analysis.
2) preparation of test solution:
Chinese prickly ash (rattan green pepper) sample is ground into powder (crossing No. three sieves) with pulverizer, 10g sample is weighed in conical flask, adds
Enter corn oil 60mL, the extracting at constant temperature 150min in 80 DEG C of thermostat water baths filters to take subsequent filtrate, draws 1mL flower with liquid-transfering gun
Green pepper extraction oil (rattan green pepper extraction oil) dissolves with isopropanol and is settled to graduation mark, oscillation shakes up, with 0.45 in 50mL volumetric flask
μm filtering with microporous membrane, take subsequent filtrate to get.
3) 5 μ L reference substance solutions and test solution injection liquid chromatograph are drawn respectively, and chromatographic condition is as follows:
Chromatographic column: Shiseido CAPCELL PAK C18Column (250mm × 4.6mm, 5 μm;MGII);30 DEG C of column temperature;Mobile phase:
Using acetonitrile as mobile phase A, using water as Mobile phase B gradient elution;Flow rate of mobile phase 1.00mL/min;Gradient elution program is as follows:
After being detected using high performance liquid chromatography, be computed obtain Chinese prickly ash (rattan green pepper) sample in hydroxyl-alpha-sanshool,
Hydroxy-beta-sanshool, hydroxyl-γ-sanshool, linalool, limonene content be shown in Table 1.
1 Chinese prickly ash of table (rattan green pepper) flavor substance content
"-" indicates to exceed detection limit
The measurement of embodiment 2 Zanthoxylum essential oil (Tengjiao oil) flavor substance
1) preparation of reference substance solution: precision weighs hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-mountain respectively
Green pepper element, linalool, limonene reference substance are dissolved with isopropanol respectively in 5 volumetric flasks and are settled to scale and obtain concentration and be
The reference substance stock solution of 8mg/mL, 0.9mg/mL, 0.8mg/mL, 20mg/mL, 10mg/mL, then 1mL mother liquor is respectively taken to hold in 10mL
The mixing reference substance of 800 μ g/mL, 90 μ g/mL, 80 μ g/mL, 2000 μ g/mL, 1000 μ g/mL are made of isopropanol constant volume for measuring bottle
Solution stores it under the conditions of -20 DEG C for liquid phase analysis.
2) preparation of test solution:
1mL Zanthoxylum essential oil is drawn in 50mL volumetric flask with liquid-transfering gun precision, is settled to graduation mark with isopropanol, oscillation shakes up
Dissolve Zanthoxylum essential oil (Tengjiao oil), with 0.45 μm of filtering with microporous membrane, take subsequent filtrate to get;
3) 5 μ L reference substance solutions and test solution injection liquid chromatograph are drawn respectively, and chromatographic condition is as follows:
Chromatographic column: Shiseido CAPCELL PAK C18Column (250mm × 4.6mm, 5 μm;MGII);30 DEG C of column temperature;Mobile phase:
Using acetonitrile as mobile phase A, using water as Mobile phase B gradient elution;Flow rate of mobile phase 1.00mL/min;Gradient elution program is as follows:
After being detected using high performance liquid chromatography, it is computed and obtains hydroxyl-alpha-sanshool, hydroxyl in Chinese prickly ash oil samples
Base-β-sanshool, hydroxyl-γ-sanshool, limonene, linalool content be shown in Table 2.
2 Zanthoxylum essential oil of table (Tengjiao oil) flavor substance content
Illustrate beneficial effects of the present invention below by way of the mode of test example:
1 chromatography condition of test example and methodological study
The selection of 1 Detection wavelength
All-wave length (190- is carried out to 3 kinds of spicy components and 2 kinds of fragrance matter standard items using ultraviolet-uisible spectrophotometer
Within the scope of 460nm) scanning, to determine maximum absorption wavelength, the result is shown in Figure 1, Fig. 2.By Fig. 1 it follows that hydroxyl-alpha-Chinese pepper
Element, hydroxy-beta-sanshool, hydroxyl-γ-sanshool have maximum absorption band in 270nm;Obtained by Fig. 2: linalool, limonene exist
200nm has maximum absorption band.
2 gradient procedure selections
Different gradient programs is set, different elution program schemes are shown in Table under 3, table 4 and table 5, variant scheme high
Effect liquid phase chromatogram figure is shown in Fig. 3 (scheme 1), Fig. 4 (scheme 2) and Fig. 5 (scheme 3).Each scheme peak separating degree situation is shown in Table 6.
3 scheme of table, 1 gradient elution program
4 scheme of table, 2 gradient elution program
5 scheme of table, 3 gradient elution program
6 different schemes gradient elution program flavor substance of table separates situation
According to the peak shape and separating degree of chromatographic peak under each gradient program, be ultimately determined to scheme 1: mobile phase is second
Nitrile-water, condition of gradient elution: 0~15min, acetonitrile-water (40:60~50:50);15~25min, acetonitrile-water (50:50~
60:40);25~35min, acetonitrile-water (60:40~70:30);35~60min acetonitrile-water (70:30), 30 DEG C of column temperature, flow velocity
1.0mL/min, 5 μ L of sample volume, Detection wavelength 200nm, 270nm.: use above-mentioned gradient elution program, 3 kinds of main spicy components
It can reach in 60min with two kinds of fragrance matters and be kept completely separate, separating degree is all larger than 1.5, and peak shape is sharp, and symmetry is good
It is good.
3 methodological studies
3.1 linear relationships are investigated
100 μ L, 200 μ L, 400 μ L, 600 μ L, 800 μ L, 1000 μ L mixing reference substance mother liquors are drawn respectively with liquid-transfering gun in 6
In a 2ml brown volumetric flask, and it is settled to graduation mark with isopropanol, is configured to the standard solution of different quality concentration.By " 2 " item
Under the conditions of sample introduction measure, high-efficient liquid phase chromatogram is shown in Fig. 3.It is repeated 3 times, respectively using peak area as ordinate (Y), mass concentration
(μ g/mL) is that abscissa (X) carries out linear regression, the results showed that each spicy component and flavor component in respective range with peak face
Product is in good linear relationship, and regression equation is detailed in the range of linearity and related coefficient, and see Table 7 for details.
7 regression equation of table, the range of linearity and related coefficient
3.2 Precision Experiment
Precision draws 5 μ L mixed reference substance solutions, and by condition under " 2 " item, sample introduction is analyzed, continuous sample introduction 6 times, measures peak face
Product, as a result the RSD of each Component peak area is hydroxyl-alpha-sanshool 0.56%, hydroxy-beta-sanshool 0.27%, hydroxyl-respectively
γ-sanshool 0.38%, linalool 0.76%, limonene 0.68% show that instrument precision is good.
3.3 stability experiment
Precision draws same Zanthoxylum essential oil test solution, according to chromatographic condition under " 2 " item, respectively at 0,4,8,12,18 and
For 24 hours sample introduction measure, measure each Component peak area RSD be respectively hydroxyl-alpha-sanshool 1.21%, hydroxy-beta-sanshool 0.86%,
Hydroxyl-γ-sanshool 0.75%, linalool 0.98%, limonene 1.07% show extracting solution interior for 24 hours basicly stable.
3.4 repetitive test
Same brand Zanthoxylum essential oil is taken to prepare 6 parts of test solutions by 3 lower section methods of embodiment, according to chromatostrip under " 2 " item
Part is measured analysis, and as a result the RSD of each composition quality score is respectively hydroxyl-alpha-sanshool 0.77%, hydroxy-beta-sanshool
0.61%, hydroxyl-γ-sanshool 0.36%, linalool 0.86%, limonene 1.01% show that the repeatability of this method is good.
The test of 3.5 sample recovery rates
Precision draws same each 0.5mL of brand Zanthoxylum essential oil of flavor substance content known to 6 parts 1 in the volumetric flask of 50mL,
Suitable hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool, linalool, limonene standard items are separately added into,
Isopropanol constant volume is used again.And lower method same treatment sample introduction 6 times according to embodiment 2, and peak area is measured respectively, calculate the rate of recovery
And RSD value.It the results are shown in Table 8.
8 flavor substance components recoveries test result of table
The verifying of the assay of 3.6 Chinese prickly ashes (rattan green pepper) and Zanthoxylum essential oil (Tengjiao oil) spicy components and fragrance matter
According to chromatographic condition under " 2 " item, to Chinese prickly ash (Hanyuan County, sichuan Province Chinese prickly ash, Hancheng Region, Shaanxi Chinese prickly ash, Gansu Wudu Chinese prickly ash), rattan
Green pepper (sichuan shantai rattan green pepper, Sichuan Jinyang pericarpium zanthoxyli schinifolii, Sichuan Hongya rattan green pepper), Zanthoxylum essential oil (bull market slope Zanthoxylum essential oil, nine bucket bowl Chinese prickly ashes
Oil, Yongfeng and Zanthoxylum essential oil), 3 kinds in 12 samples of Tengjiao oil (pockmarks Tengjiao oil, ten thousand not Tengjiao oil, bull market slope Tengjiao oil)
Main spicy component and 2 kinds of Main Fragrances are carried out while being measured, and Chinese prickly ash (oil) high-efficient liquid phase chromatogram is shown in Fig. 6, rattan green pepper
(oil) high-efficient liquid phase chromatogram result is shown in Fig. 7, and measurement result is the same as the table 2 in the table 1 and embodiment 2 in embodiment 1.
Result by chromatography condition and methodological study is visible: the detection method can be used for measuring Chinese prickly ash simultaneously
Chemical component hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, the hydroxyl-γ-of " fiber crops " in (oil) and/or rattan green pepper (oil) flavor substance
Sanshool, and chemical component limonene, the linalool of " perfume ".As a result reliable, to the quality of Chinese prickly ash (rattan green pepper) and its Related product
Control and scientific evaluation are of great significance, and have a good application prospect.
Claims (10)
1. a kind of method for measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product simultaneously, it is characterised in that: it is to use
High performance liquid chromatography detection, operating procedure are as follows:
1) hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool, limonene, virtue the preparation of reference substance solution: are taken
Camphor tree alcohol reference substance, adds isopropanol to dissolve, freezen protective, as reference substance solution;
2) preparation of test solution:
A Chinese prickly ash or rattan green pepper test sample: taking test sample to crush, and sieving adds edible oil extract, filters, and extracting solution adds isopropanol to dissolve,
Filtering, takes filtrate as test solution;
B Zanthoxylum essential oil or Tengjiao oil test sample: taking test sample, isopropanol added to dissolve, and filtering takes filtrate as test solution;
3) reference substance solution being drawn respectively and test solution injecting liquid chromatograph, chromatographic condition is as follows:
Chromatographic column: using octadecylsilane chemically bonded silica as filler;Mobile phase: using acetonitrile as mobile phase A, using water as mobile phase
B gradient elution;Gradient elution program is as follows:
2. detection method according to claim 1, it is characterised in that: the step 1) reference substance solution hydroxyl-α-mountain
Green pepper element, hydroxy-beta-sanshool, hydroxyl-γ-sanshool, limonene, linalool concentration be respectively 800ug/mL, 90ug/mL,
80ug/mL、2000ug/mL、1000ug/mL。
3. detection method according to claim 1, it is characterised in that: the step 1) cryogenic temperature is -20 DEG C.
4. detection method according to claim 1, it is characterised in that: the sieve of sieving described in step a is No. three sieves.
5. detection method according to claim 1, it is characterised in that: Chinese prickly ash described in step a or rattan green pepper sample to be tested and food
Mass volume ratio with oil is 10g:60mL, and the edible oil is corn oil.
6. detection method according to claim 1, it is characterised in that: be extracted as extracting at constant temperature, extraction time described in step a
For 150min, extraction temperature is 80 DEG C.
7. detection method according to claim 1, it is characterised in that: the volume ratio of extracting solution described in step a and isopropanol
For 1:50;The volume ratio of Zanthoxylum essential oil described in step b or Tengjiao oil sample to be tested and isopropanol is 1:50.
8. detection method according to claim 1, it is characterised in that: be injected separately into liquid chromatograph described in step 3)
Reference substance solution and test solution amount are 5 μ l.
9. detection method according to claim 1, it is characterised in that: step 3) the octadecylsilane chemically bonded silica color
Compose column are as follows: Shiseido CAPCELL PAK C18 column, 250mm × 4.6mm, 5 μm, MGII.
10. detection method according to claim 1, it is characterised in that: flow velocity is in the step 3) chromatographic condition
1.00ml/min, column temperature are 30 DEG C, wavelength 200nm, 270nm.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811533692.0A CN109444284B (en) | 2018-12-14 | 2018-12-14 | Method for simultaneously determining flavor substances in pepper and/or rattan pepper and oil products thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811533692.0A CN109444284B (en) | 2018-12-14 | 2018-12-14 | Method for simultaneously determining flavor substances in pepper and/or rattan pepper and oil products thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109444284A true CN109444284A (en) | 2019-03-08 |
CN109444284B CN109444284B (en) | 2021-09-24 |
Family
ID=65559552
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811533692.0A Active CN109444284B (en) | 2018-12-14 | 2018-12-14 | Method for simultaneously determining flavor substances in pepper and/or rattan pepper and oil products thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109444284B (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112683832A (en) * | 2020-12-18 | 2021-04-20 | 广电计量检测(成都)有限公司 | Method for detecting numb-taste substances in fresh pepper |
CN112684068A (en) * | 2020-12-21 | 2021-04-20 | 苏州华测生物技术有限公司 | Method for measuring content of hydroxy-alpha-sanshool |
CN112881561A (en) * | 2021-01-22 | 2021-06-01 | 四川省食品药品检验检测院(四川省药品质量研究所、四川省医疗器械检测中心) | System and method for determining sanshool in rattan pepper |
CN113777190A (en) * | 2021-08-27 | 2021-12-10 | 重庆市日用化学工业研究所 | Method for separating and measuring sanshool content in pepper extract and pepper extract product and application of sanshool content |
CN113917039A (en) * | 2021-10-27 | 2022-01-11 | 甘肃奇正藏药有限公司 | Method for measuring content of effective components in pepper and products thereof |
CN114062545A (en) * | 2021-11-15 | 2022-02-18 | 幺麻子食品股份有限公司 | Method for identifying authenticity of zanthoxylum schinifolium oil by taking tingling taste as index |
CN116808106A (en) * | 2023-05-23 | 2023-09-29 | 成都中医药大学 | Zanthoxylum bungeanum volatile oil liposome |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102690208A (en) * | 2012-05-31 | 2012-09-26 | 四川大学 | Method for extracting hydroxyl sanshool from zanthoxylum oil |
JP2015027309A (en) * | 2014-09-30 | 2015-02-12 | 太一 染谷 | Agent for imparting beer flavor, and beer-flavored beverage |
CN107966514A (en) * | 2017-11-28 | 2018-04-27 | 晨光生物科技集团股份有限公司 | The detection method of numb-taste component of zanthoxylum content in a kind of pepper extract |
US20180224411A1 (en) * | 2015-07-31 | 2018-08-09 | Scientific Holdings, Llg | Botanical identification method and system |
-
2018
- 2018-12-14 CN CN201811533692.0A patent/CN109444284B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102690208A (en) * | 2012-05-31 | 2012-09-26 | 四川大学 | Method for extracting hydroxyl sanshool from zanthoxylum oil |
JP2015027309A (en) * | 2014-09-30 | 2015-02-12 | 太一 染谷 | Agent for imparting beer flavor, and beer-flavored beverage |
US20180224411A1 (en) * | 2015-07-31 | 2018-08-09 | Scientific Holdings, Llg | Botanical identification method and system |
CN107966514A (en) * | 2017-11-28 | 2018-04-27 | 晨光生物科技集团股份有限公司 | The detection method of numb-taste component of zanthoxylum content in a kind of pepper extract |
Non-Patent Citations (4)
Title |
---|
JOHANNA RUDBACK等: "A sensitive method for determination of allergenic fragrance terpene hydroperoxides using liquid chromatography coupled with tandem mass spectrometry", 《JOURNAL OF SEPARATION SCIENCE》 * |
XIAOGEN YANG: "Aroma Constituents and Alkylamides of Red and Green Huajiao (Zanthoxylum bungeanum and Zanthoxylum schinifolium)", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
何祖新 等: "日本无刺花椒风味物质的分析研究", 《中国调味品》 * |
张丽平 等: "花椒中柠檬烯和芳樟醇的含量测定与比较分析", 《中国调味品》 * |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112683832A (en) * | 2020-12-18 | 2021-04-20 | 广电计量检测(成都)有限公司 | Method for detecting numb-taste substances in fresh pepper |
CN112684068A (en) * | 2020-12-21 | 2021-04-20 | 苏州华测生物技术有限公司 | Method for measuring content of hydroxy-alpha-sanshool |
CN112881561A (en) * | 2021-01-22 | 2021-06-01 | 四川省食品药品检验检测院(四川省药品质量研究所、四川省医疗器械检测中心) | System and method for determining sanshool in rattan pepper |
CN113777190A (en) * | 2021-08-27 | 2021-12-10 | 重庆市日用化学工业研究所 | Method for separating and measuring sanshool content in pepper extract and pepper extract product and application of sanshool content |
CN113917039A (en) * | 2021-10-27 | 2022-01-11 | 甘肃奇正藏药有限公司 | Method for measuring content of effective components in pepper and products thereof |
CN114062545A (en) * | 2021-11-15 | 2022-02-18 | 幺麻子食品股份有限公司 | Method for identifying authenticity of zanthoxylum schinifolium oil by taking tingling taste as index |
CN116808106A (en) * | 2023-05-23 | 2023-09-29 | 成都中医药大学 | Zanthoxylum bungeanum volatile oil liposome |
CN116808106B (en) * | 2023-05-23 | 2024-03-01 | 成都中医药大学 | Zanthoxylum bungeanum volatile oil liposome |
Also Published As
Publication number | Publication date |
---|---|
CN109444284B (en) | 2021-09-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109444284A (en) | Method that is a kind of while measuring flavor substance in Chinese prickly ash and/or rattan green pepper and its oil product | |
CN102608244A (en) | Detection method for simultaneously determining several kinds of fragrant substances in cigarette tobacco shreds | |
Li et al. | Simultaneous determination of terpene lactones and flavonoid aglycones in Ginkgo biloba by high-performance liquid chromatography with evaporative light scattering detection | |
CN106525997A (en) | Method for determination of organic acids and flavone components in polygonum viviparum | |
CN104569279A (en) | Quality detection method of inflammation diminishing and pain easing ointment | |
CN103760278A (en) | High efficiency liquid chromatography method for simultaneously quantitatively detecting six flavonoid components in polygonum hydropiper | |
CN106353417A (en) | UPLC (ultra-performance liquid chromatography) detection method of multiple steroid saponins in Yunnan rhizoma paridis or its polygerm strain | |
CN107037167A (en) | The method of flavones ingredient content in multi-target ingredient quantitative determination ginkgo leaf | |
Hong et al. | Determination of indole alkaloids and highly volatile compounds in Rauvolfia verticillata by HPLC–UV and GC–MS | |
CN109765322A (en) | The characteristic spectrum construction method and quality determining method of schizonepeta | |
CN104330482B (en) | A kind of HPLC of utilization measures the method for 17 kinds of characteristic components in Folium Camelliae sinensis simultaneously | |
CN114527218A (en) | Method for detecting components of scutellaria baicalensis | |
CN105158355B (en) | Method for rapidly measuring content of four spermidine ingredients in carthamus tinctorius simultaneously | |
CN110133153A (en) | Method that is a kind of while measuring 5 kinds of chemical composition contents in chrysanthemum medicinal material | |
CN109490446A (en) | Method that is a kind of while measuring 5 kinds of flavone compounds in ground centipede medicinal material | |
CN109324127A (en) | The detection method of taxol in Chinese yew extract | |
CN114034798B (en) | Red water dendrobium stem flower fingerprint construction and content determination method | |
CN1853674B (en) | Quality controlling method of Xingdan injection | |
CN104597168B (en) | Ramulus Mori refines decoction pieces content assaying method | |
CN103048347B (en) | Method for distinguishing root-bark medicinal materials of celastrus angulatus | |
CN109917048A (en) | A kind of construction method of the UPLC characteristic spectrum of bark of ash medicinal material, the characteristic spectrum constructed by this method and its application | |
CN107976498A (en) | A kind of detection method of yellow angledtwig magnoliavine root stem and leaf functionality active component and application | |
CN108918721A (en) | A kind of measuring method of tussilago Content of Chlorogenic Acid | |
CN103399089B (en) | Method for measuring eugenol in edible flavour and fragrance based on high performance liquid chromatography | |
Wang et al. | HPLC fingerprint combined with quantitation of main effective components and chemometrics as an efficient method for quality evaluation of Oviductus Ranae |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |