CN106770788A - Numb-taste components content detection based on " one surveys comment more " method - Google Patents
Numb-taste components content detection based on " one surveys comment more " method Download PDFInfo
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- CN106770788A CN106770788A CN201710024850.9A CN201710024850A CN106770788A CN 106770788 A CN106770788 A CN 106770788A CN 201710024850 A CN201710024850 A CN 201710024850A CN 106770788 A CN106770788 A CN 106770788A
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- sanshool
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- 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
Abstract
The invention discloses the numb-taste components content detection based on " one surveys comment more " method, comprise the following steps：(1) foundation of hydroxyl β sanshools standard curve：(2) in testing sample hydroxyl β sanshools assay：(3) hydroxyl α sanshools and hydroxyl γ Chinese pepper cellulose contents in relative correction factor calculating testing sample are used." one surveys comment more " method of the invention is mutually authenticated with external standard method, no significant difference, reliable results.The present invention overcomes in the case where hydroxyl α sanshools and hydroxyl γ sanshool reference substances is lacked by relative correction factor f and chromatographic peak location Calculation its content, main spicy components hydroxyl α sanshools composition and hydroxyl γ sanshool quality controls in Chinese prickly ash are realized, for the quality control of Chinese prickly ash provides new method.
Description
Technical field
Numb-taste components content detection the present invention relates to be based on " one surveys comment more " method.
Background technology
The spicy components of Chinese prickly ash are concentrated mainly on the oil droplet cell of Chinese prickly ash pericarp, and research shows, the unsaturated lipid in Chinese prickly ash
Fat acid acid amides constituents are the spicy components in Chinese prickly ash.At present, existing scholar identifies 25 kinds of spicy components from Chinese prickly ash, wraps
Include α-sanshool, β-sanshool, γ-sanshool, hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool etc..Its
In, hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool is topmost spicy components in Chinese prickly ash.
The numb taste of Chinese prickly ash is one of main form of expression of Chinese prickly ash quality evaluation, at present still without commercially available Chinese prickly ash fiber crops taste
Material reference substance, and existing Chinese prickly ash national standard and provincial standard do not carry out objective quantitative to the numb taste of Chinese prickly ash.
Therefore, it is necessary to separated to spicy component in Chinese prickly ash, by determine simultaneously multiple spicy components indexs into
Point, realize to the spicy components content detection in Chinese prickly ash.
The content of the invention
To solve the above problems, the present invention provides the numb-taste components content detection based on " one surveys comment more " method, including
Following steps：
(1) foundation of hydroxy-beta-sanshool standard curve：
The preparation of a, reference substance solution：
Hydroxy-beta-sanshool reference substance is taken, plus methyl alcohol is configured to reference substance solution；
The measure of b, reference substance solution：
The reference substance solution of series concentration is prepared, high performance liquid chromatograph is injected separately into, each chromatographic peak peak area is determined, obtained
To the standard curve of hydroxy-beta-sanshool；
Chromatographic condition is as follows：
Detection wavelength：270±5nm；
Chromatographic column：C18Chromatographic column；
Mobile phase：Acetonitrile：Water=40%：60%；
(2) in testing sample hydroxy-beta-sanshool assay：
The preparation of c, need testing solution：
Testing sample is taken, plus methyl alcohol is extracted, and filters to obtain need testing solution；
The measure of d, need testing solution：
Need testing solution is taken, high performance liquid chromatograph is injected, is detected with step b identicals chromatographic condition, according to step (1)
Standard curve obtain the content of hydroxy-beta-sanshool in testing sample；
(3) hydroxyl-alpha-sanshool and hydroxyl-γ-Chinese pepper cellulose content in relative correction factor calculating testing sample are used.
Further, the C18Chromatographic column is Phenomenex C18Chromatographic column, Waters Bridge C18Or Agilent
Eclipse Plus C18Chromatographic column.
Further, the specification of the chromatographic column is 250mm × 4.6mm, 5 μm.
Further, the high performance liquid chromatograph is Agilent 1260, Shimadzu LC-2010A or Waters e2695.
Further, in step c, the extraction is ultrasonic extraction.
Further, the time of the ultrasonic extraction is 30 minutes.
Further, in step c, the methyl alcohol is 100mL with the volume mass ratio of testing sample：1g.
Further, the column temperature of the chromatographic condition is 20~30 DEG C, preferably 30 DEG C.
Further, the flow velocity of the chromatographic condition is 0.6~1.0mLmin-1, preferably 1.0mLmin-1。
Further, the relative correction factor of the step (3) is obtained by following step：
Hydroxyl-alpha-sanshool, hydroxyl-γ-sanshool and hydroxy-beta-sanshool reference substance are taken, plus methyl alcohol is configured to mixing
Reference substance solution；
Mixed reference substance solution is taken, high performance liquid chromatograph is injected, is detected with step b identicals chromatographic condition, obtain hydroxyl
The standard curve of base-α-sanshool, hydroxyl-γ-sanshool and hydroxy-beta-sanshool；
It is internal reference thing with hydroxy-beta-sanshool, according to relative response factor f computing formula：Calculating hydroxyl-alpha-sanshool,
The corresponding factor between hydroxyl-γ-sanshool and hydroxy-beta-sanshool, takes its average；
Wherein, relative response factor f computing formula are as follows：
The mass concentration that A is chromatographic peak area in formula, W is composition, subscript n represents composition to be measured, subscript behalf internal reference
Thing.
It is used to detect Chinese prickly ash, Zanthoxylum essential oil, rattan green pepper, Tengjiao oil and products thereof present invention also offers content detection of the invention
The content detection of middle spicy components.
Tests prove that, chromatographic condition of the present invention can effectively by hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, and hydroxyl-
γ-sanshool is separated, so that Accurate Determining their content.Also, " one surveys comment more " method of the invention is mutually tested with external standard method
Card, no significant difference, reliable results.
In addition, inventor separates the hydroxy-beta-sanshool reference substance for preparing authorized by middle inspection, can be as flower
The reference substance of green pepper is used.Lacking hydroxyl-alpha-sanshool and hydroxyl-γ-sanshool control so as to the inventive method can overcome
By relative correction factor f and chromatographic peak location Calculation its content in the case of product, realize main spicy components hydroxyl in Chinese prickly ash-
α-sanshool composition and hydroxyl-γ-sanshool quality control, for the quality control of Chinese prickly ash provides new method.Therefore, this hair
Bright method can be used for the detection of Chinese prickly ash, rattan green pepper and products thereof.
Obviously, the above of the invention, according to the ordinary technical knowledge and customary means of this area, is not departing from
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification of other diversified forms can also be made, is replaced or is changed.
The specific embodiment of form, remakes further specifically to the above of the invention by the following examples
It is bright.But this scope for being interpreted as above-mentioned theme of the invention should not be only limitted to following example.It is all based on the above of the present invention
The technology realized belongs to the scope of the present invention.
Brief description of the drawings
Fig. 1 is mixed reference substance solution HPLC chromatogram (1-hydroxyl-alpha-sanshool；2-hydroxy-beta-sanshool；3-hydroxyl
Base-γ-sanshool)
Fig. 2 is need testing solution HPLC chromatogram (1-hydroxyl-alpha-sanshool；2-hydroxy-beta-sanshool；3-hydroxyl-
γ-sanshool)
Specific embodiment
Embodiment 1
1 instrument
The high performance liquid chromatographs of Agilent 1260, G1311C quaternary pumps, G1329B automatic samplers, G1316A column temperatures
Case, G1362A PDADs (Agilent companies of the U.S.)；Waters e2695 high performance liquid chromatographs, quaternary pump,
2998PDA detectors；Shimadzu Shimadzus LC-2010A, SIL-20A automatic sampler, SPD-20A detectors, CTO-20A posts
Incubator, LC solution chromatographic work stations software (Japanese Shimadzu Corporation)；BP211D electronic analytical balances (German Sartouris
Limited company).
2 materials and reagent
Chinese prickly ash：Hanyuan County, sichuan Province Chinese prickly ash office provides.
Numb-taste components reference substance：Hydroxyl-alpha-sanshool (self-control, purity 98.35%)；Hydroxy-beta-sanshool (from
System, applies for into national reference substance, purity 98.27%)；Hydroxyl-γ-sanshool (self-control, purity 98.54%).
Methyl alcohol：Chromatographic grade, sigma companies of the U.S..Acetonitrile：Chromatographic grade, sigma companies of the U.S..
3 HPLC chromatogram conditions
Chromatographic column Phenomenex C18Post (250mm × 4.6mm, 4 μm)；With acetonitrile (A)：Water (B)=40%：60% is
Mobile phase, isocratic elution 45min, column flow 1.0min/mL, Detection wavelength 270nm, 30 DEG C of column temperature, the μ L of sample size 10.
4 one survey the foundation for commenting method more
The determination of 4.1 relative correction factors
4.1.1 the preparation of mixed reference substance solution
Accurately weighed hydroxyl-alpha-the sanshool of difference, hydroxy-beta-sanshool, hydroxyl-γ-sanshool reference substance is placed in right amount
In 100mL volumetric flasks, plus methanol constant volume is to scale, is made into mass concentration respectively 1.70mg/mL, 0.475mg/mL,
The reference substance solution of 0.189mg/mL, as reference substance stock solution.Precision draws above-mentioned each 1mL of reference substance storing solution, puts
In 10mL volumetric flasks, plus methanol constant volume is to scale, shakes up, and is made into interstitial fluid in reference substance.Then, precision pipettes above-mentioned control respectively
Each 2mL of interstitial fluid in product, in putting 10mL volumetric flasks, plus methanol constant volume is to scale, shakes up, and is made into mixed reference substance solution.Will be above-mentioned
Mixed reference substance solution be stored in it is standby in 4 DEG C of refrigerators, it is standby.
4.1.2 prepared by need testing solution
Precision weighs zanthoxylum powder (crossing No. four sieves) about 0.5g and is accurate to (0.0001g), puts in conical flask with cover, adds 50mL
Methyl alcohol, obtains final product after sonic oscillation 30min filterings.It is accurate respectively to draw above-mentioned reference substance solution and each 10 μ L of need testing solution, note
Enter liquid chromatograph, determine, as a result see Fig. 1, Fig. 2.
4.1.3 linear, quantitative limit and test limit
It is accurate respectively to draw the 4.1.1 lower μ L sample introductions analysis of mixed reference substance solution 2,5,10,15,20,25,30, with peak
Area is ordinate, and sample introduction concentration is abscissa, draws standard curve；With the reference substance solution stepwise dilution of least concentration, point
Not using concentration that signal to noise ratio is 3 and 10 as test limit and quantitative limit, 1 is shown in Table.
The linear relationship of table 1 and quantitative limit, test limit
4.1.4 the calculating of relative correction factor
Under the conditions of the HPLC chromatogram analysis determined under " 2 " item, the mixing reference substance that precision is drawn under " 4.1.1 " item is molten
Liquid, difference sample introduction 2,5,10,15,20,25,30 μ L.It is internal reference thing with hydroxy-beta-sanshool, is counted according to relative response factor (f)
Formula (1) is calculated, hydroxyl-alpha-sanshool, the corresponding factor between hydroxyl-γ-sanshool and hydroxy-beta-sanshool is calculated, taken
Its average.
The mass concentration of A, W in formula, respectively chromatographic peak area, composition, subscript n, s represents composition to be measured and internal reference respectively
Thing.The results are shown in Table 2, should under the conditions of result of calculation relative correction factor value for f hydroxyl-alphas-sanshool/hydroxy-beta-sanshool=
1.0238, RSD is 0.87%；F hydroxyls-γ-sanshool/hydroxy-beta-sanshool=0.7986, RSD show difference for 0.54%
Relative correction factor under sampling volume is relatively stable.
Relative correction factor under the different sampling volumes of table 2
4.1.5 precision test
Precision pipettes mixed reference substance solution under " 4.1.1 " item, continuous sample introduction 6 times, and 10 μ L, record each composition respectively every time
Peak area simultaneously calculates its RSD, as a result hydroxyl-alpha-sanshool, and hydroxy-beta-sanshool, the RSD values of hydroxyl-γ-sanshool are respectively
0.16%, 0.11%, 0.32%, show that instrument precision is good.
4.1.6 replica test
Precision is weighed with a collection of Pricklyash peel about 0.5g, and by 3.1.2 lower operation, 6 parts of need testing solutions of parallel preparation are surveyed
Hydroxyl-alpha-sanshool is obtained, hydroxy-beta-sanshool, the content RSD of hydroxyl-γ-sanshool is respectively 0.02%, 0.42%,
0.29.Show that sample repeatability is good.
4.1.7 stability test
Precision draws the same μ L of mixed reference substance solution 10, and respectively at 0,2,4,6,8,12,24,36h sample introductions are determined respectively
Hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, the peak area of hydroxyl-γ-sanshool, the RSD of its peak area is respectively 0.25%,
0.27%, 0.47.Show that the mixed reference substance solution is good in 36h internal stabilities.
4.1.8 it is loaded recovery test
Take with the Pricklyash peel 0.25g of a collection of known content, it is accurately weighed, parallel 6 parts, respectively it is accurate add hydroxyl-alpha-
Sanshool, hydroxy-beta-sanshool, hydroxyl-γ-sanshool reference substance stock solution is surveyed by need testing solution is prepared under 4.1.2
It is fixed, hydroxyl-alpha-sanshool is calculated, hydroxy-beta-sanshool, the average recovery of hydroxyl-γ-sanshool the results are shown in Table 3.
Hydroxyl-alpha-sanshool in the Chinese prickly ash of table 3, hydroxy-beta-sanshool, the average recovery experiment knot of hydroxyl-γ-sanshool
Really
4.2 1 surveys comments method system robustness and system suitability
4.2.1 the durability and system suitability of relative correction factor
Agilent 1260, the highly effective liquid phase chromatographic system of Shimadzu LC-2010A and Agilent 1200 are selected in this experiment respectively
With Agilent Eclipse Plus C18(4.6mm × 250mm, 5 μm), Waters Bridge C18(4.6mm × 250mm, 5 μ
And Phenomenex C m)18(4.6mm × 250mm, 5 μm) 3 kinds of chromatographic columns, investigate shadow of the chromatographic system to relative correction factor
Ring.Result shows that different chromatographic systems influence smaller (RSD ＜ 5.0%) on it, and reappearance is good, is shown in Table 4.
Influence of the different chromatographic systems of table 4 to relative correction factor
4.2.2 the positioning of component chromatographic peak to be measured
4.2.2.1 different instruments and chromatographic column are to relative retention time
According to the retention time of hydroxy-beta-sanshool, the phase using hydroxyl-alpha-sanshool relative to hydroxy-beta-sanshool
To retention time r, formula (2) is seen, you can peak is positioned.
R=rx/rs (2)
Wherein rx, rsThe retention time of determinand and internal reference thing is represented respectively.
Experiment has investigated relative retention time value in different brands chromatograph, the reappearance of different brands chromatographic column respectively,
The results are shown in Table 5.Result shows that retention time change of the different chromatographic columns to each composition is more apparent, but relative reservation between each composition
Less, RSD ＜ 5.0%, the retention time change of same model chromatographic column each composition on different instruments is little for value changes.Therefore,
This experiment is more suitable as the positioning index of target chromatographic peak from relative retention value.
Table 5 one surveys the positioning for commenting method composition chromatographic peak to be measured more
4.2.2.2 different in flow rate and column temperature is to relative retention time
Under the same conditions, using the chromatographic systems of Agilent 1260 and Waters Bridge C18Chromatographic column is investigated respectively
It is different in flow rate (0.6,0.8,1.0mLmin- 1) and different column temperatures (20,25,30 DEG C) to hydroxyl-alpha-sanshool, hydroxy-beta-mountain
The influence of the relative retention time of green pepper element, as a result shows smaller (the RSD ＜ of influence of the different in flow rate, column temperature to relative retention time
3.0%).
4.3 " one surveys comment more " method external standard methods compare
First using external standard method to hydroxyl-alpha-sanshool in Chinese prickly ash, hydroxy-beta-sanshool, hydroxyl-γ-sanshool is carried out
Determine, resettle and comment method to be calculated a survey more, and the result that two methods are calculated is compared, comment method a survey more to verify
To the accuracy for determining spicy components evaluation in Chinese prickly ash.Result shows, the numb-taste components content that two methods are measured
There was no significant difference, points out the method set up to have preferable confidence level.The results are shown in Table 6.
The external standard method of table 6 and one surveys the comparings for commenting method to determine hydroxyl-alpha-Chinese pepper cellulose content in Chinese prickly ash more
5 discuss
5.1 Detection wavelengths
Efficient liquid phase DAD detectors are selected in this experiment, to the hydroxyl-alpha-sanshool for preparing under 190~400nm, hydroxyl-
β-sanshool, hydroxyl-γ-sanshool reference substance have carried out full wavelength scanner.Result shows hydroxyl-alpha-sanshool, hydroxy-beta-mountain
Green pepper element, hydroxyl-γ-sanshool reference substance absorption maximum is respectively in 272nm, 267nm, 270nm, place.In view of hydroxyl-γ-mountain
Green pepper cellulose content is minimum, therefore selects its absorption maximum 270nm as Detection wavelength.
The selection of 5.2 internal reference things
This experiment is internal reference thing from hydroxy-beta-sanshool, is easy to get because prepared by its reference substance, and physicochemical property is relatively stable,
Can for a long time preserve and use, checked approval by middle inspection uses as Chinese prickly ash reference substance.
The selection of 5.3 chromatographic conditions
Hydroxyl-alpha-sanshool, hydroxy-beta-sanshool are cis-trans isomer, and property is similar, more difficult separation.The author
The flow phase systems such as trial methanol-water, acetonitrile-water, methanol-water-formic acid, acetonitrile-water-formic acid are under conditions of isocratic elution
To hydroxyl-alpha-sanshool, hydroxy-beta-sanshool, the separation of hydroxyl-γ-sanshool is investigated, as a result show using acetonitrile-
Water system (40:60) isocratic elution is carried out, analysis time is shorter, two compositions can reach desired separated, and peak shape is good.Therefore
It is final to use acetonitrile-water system (40:60) isocratic elution is carried out as mobile phase.
5.4 interpretations of result
The present invention has measured spicy components hydroxyl-alpha-sanshool in 12 batches of Chinese prickly ash samples, hydroxy-beta-sanshool, and hydroxyl-
The content of γ-sanshool." one surveys comment more " method that the present invention is used is mutually authenticated with external standard method, no significant difference, reliable results.
The inventive method can be overcome in the case where hydroxyl-alpha-sanshool and hydroxyl-γ-sanshool reference substance is lacked by relative school
Positive divisor f and chromatographic peak location Calculation its content, realize main spicy components hydroxyl-alpha-sanshool composition and hydroxyl in Chinese prickly ash-
γ-sanshool quality control." one surveys comment more " method that the present invention sets up is for the quality control of Chinese prickly ash provides new method.
Claims (11)
1. the numb-taste components content detection of " one surveys comments more " method is based on, it is characterised in that：Comprise the following steps：
(1) foundation of hydroxy-beta-sanshool standard curve：
The preparation of a, reference substance solution：
Hydroxy-beta-sanshool reference substance is taken, plus methyl alcohol is configured to reference substance solution；
The measure of b, reference substance solution：
The reference substance solution of series concentration is prepared, high performance liquid chromatograph is injected separately into, each chromatographic peak peak area is determined, hydroxyl is obtained
The standard curve of base-β-sanshool；
Chromatographic condition is as follows：
Detection wavelength：270±5nm；
Chromatographic column：C18Chromatographic column；
Mobile phase：Acetonitrile：Water=40%：60%；
(2) in testing sample hydroxy-beta-sanshool assay：
The preparation of c, need testing solution：
Testing sample is taken, plus methyl alcohol is extracted, and filters to obtain need testing solution；
The measure of d, need testing solution：
Need testing solution is taken, high performance liquid chromatograph is injected, is detected with step b identicals chromatographic condition, according to the mark of step (1)
Directrix curve obtains the content of hydroxy-beta-sanshool in testing sample；
(3) hydroxyl-alpha-sanshool and hydroxyl-γ-Chinese pepper cellulose content in relative correction factor calculating testing sample are used.
2. content detection according to claim 1, it is characterised in that：The C18Chromatographic column is Phenomenex C18Chromatogram
Post, Waters Bridge C18Or Agilent Eclipse Plus C18Chromatographic column.
3. content detection according to claim 2, it is characterised in that：The specification of the chromatographic column is 250mm × 4.6mm, 5
μm。
4. the content detection according to claim any one of 1-3, it is characterised in that：The high performance liquid chromatograph is
Agilent 1260, Shimadzu LC-2010A or Waters e2695.
5. content detection according to claim 1, it is characterised in that：In step c, the extraction is ultrasonic extraction.
6. content detection according to claim 4, it is characterised in that：The time of the ultrasonic extraction is 30 minutes.
7. content detection according to claim 1, it is characterised in that：In step c, the volume of the methyl alcohol and testing sample
Mass ratio is 100mL：1g.
8. the content detection according to claim any one of 1-7, it is characterised in that：The column temperature of the chromatographic condition be 20~
30 DEG C, preferably 30 DEG C.
9. the content detection according to claim any one of 1-8, it is characterised in that：The flow velocity of the chromatographic condition is 0.6
~1.0mLmin-1, preferably 1.0mLmin-1。
10. the content detection according to claim any one of 1-9, it is characterised in that：The relative correction of the step (3) because
Son is obtained by following step：
Hydroxyl-alpha-sanshool, hydroxyl-γ-sanshool and hydroxy-beta-sanshool reference substance are taken, plus methyl alcohol is configured to mixing control
Product solution；
Take mixed reference substance solution, inject high performance liquid chromatograph, detected with step b identicals chromatographic condition, obtain hydroxyl-alpha-
The standard curve of sanshool, hydroxyl-γ-sanshool and hydroxy-beta-sanshool；
It is internal reference thing with hydroxy-beta-sanshool, according to relative response factor f computing formula：Calculating hydroxyl-alpha-sanshool, hydroxyl-
The corresponding factor between γ-sanshool and hydroxy-beta-sanshool, takes its average；
Wherein, relative response factor f computing formula are as follows：
The mass concentration that A is chromatographic peak area in formula, W is composition, subscript n represents composition to be measured, subscript behalf internal reference thing.
Content detection described in 11. claim 1-10 any one be used to detecting Chinese prickly ash, Zanthoxylum essential oil, rattan green pepper, Tengjiao oil and its
The content detection of spicy components in product.
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| CN114062526A (en) * | 2020-08-05 | 2022-02-18 | 汉义生物科技（北京）有限公司 | Detection method for quantifying cannabinoids based on relative correction factor method |
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| 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 |
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| CN114062526B (en) * | 2020-08-05 | 2024-03-08 | 汉义生物科技（北京）有限公司 | Detection method for quantifying cannabinoid compounds based on relative correction factor method |
| 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 |
| CN113841745A (en) * | 2021-01-28 | 2021-12-28 | 丰益(上海)生物技术研发中心有限公司 | Zanthoxylum oil, preparation method and application thereof, and material using zanthoxylum oil |
| 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 |
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Application publication date: 20170531 |