CN103743842A - Method for constructing and using Guilin brine HPLC (High Performance Liquid Chromatography) fingerprint spectrums - Google Patents
Method for constructing and using Guilin brine HPLC (High Performance Liquid Chromatography) fingerprint spectrums Download PDFInfo
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- CN103743842A CN103743842A CN201410033573.4A CN201410033573A CN103743842A CN 103743842 A CN103743842 A CN 103743842A CN 201410033573 A CN201410033573 A CN 201410033573A CN 103743842 A CN103743842 A CN 103743842A
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Abstract
The invention relates to a method for constructing a Guilin brine HPLC (High Performance Liquid Chromatography) fingerprint spectrum. The method comprises the following steps: 1, preparing a sample, to be specific, taking appropriate Guilin brine, adding n-butyl alcohol, conducting ultrasonic extraction, shaking well, standing, taking supernate for spin steaming to be dry, using methanol to dissolve after methanol elution and blowing dry, and filtering with a micro-filtration membrane to obtain the sample; 2, adopting XB-C18 chromatographic columns 250 mm*4.6mm, 5 [mu]L, using methanol and water as a mobile phase, and conducting gradient elution to obtain the Guilin brine HPLC fingerprint spectrum. A Guilin brine product is determined with the same method, the obtained spectrum is compared with a standard fingerprint spectrum, whether the size of similarity conforms to the requirement or not is used as the standard for judging whether the quality of product is qualified or not. The method has higher precision, repeatability and stability and is simple and convenient for operation, the separation of spectrum and characteristic peak is better, the quality condition of Guilin brine can be grasped through the overall characteristics of the spectrum, and therefore the spectrum can be used as an index of controlling the quality of Guilin brine.
Description
Technical field
The present invention relates to a kind of construction method of flavouring finger-print, particularly structure and the using method of a kind of Guilin bittern HPLC finger-print.
Background technology
Guilin bittern is a kind of traditional condiment that has local characteristic in Guangxi, and its application is very extensive, as the seasoning of Guilin characteristic snack Guilin rice-flour noodle, and the making of stewed meat products, the stew in soy sauce of various livestock and poultry secondary products etc.Guilin bittern production method added clear water before this in pot, then add the spices such as Chinese prickly ash, anise, cassia bark, cloves, Radix Glycyrrhizae and condiments (salt, sugar, soy sauce etc.), boil approximately some hours with the little fire of the boiled rear use of big fire, finally remove to expect slag, obtain delicious bittern Normal juice, each businessman of raw material and ratio thereof is close not unofficial biography all.
The difference of bittern is the different bigger differences that cause local flavor of spice proportioning because adding often, producer is mainly to complete by master craftsman's sensory evaluation or by simple physics and chemistry detection (as salinity, sugar, acidity etc.) to the quality assessment of Guilin bittern now, but simple physical and chemical index detects and cannot reflect to a certain extent the difference between bittern, utilize the method for sensory evaluation no doubt to have very large rationality and necessity, but the instability of human factor has restricted again the science of this kind of method to a certain extent.Therefore,, on the basis of sensory evaluation and physics and chemistry detection, searching out science, effectively method for evaluating quality and means has become objective requirement.Along with the megatrend of modern food industry industrialization development, food is carried out to standardized production imperative.Therefore, enterprise need to carry out standardization to Guilin bittern, need to have a set of rational Quality Evaluation Model to carry out quality control to it.
Fingerprint pattern technology is a kind of traditional Chinese medicine quality control device that developed recently gets up, and existing traditional Chinese medicine quality control model is exactly that foreign chemicals quality control model is set up.The feature of fingerprint pattern technology is to characterize all sidedly a complex system, and its effect in medicine quality evaluated may be summarized to be: 1. observe the global feature of finger-print to differentiate the true and false of producing front medicinal material; 2. distinguish the different parts of vegetable drug; 3. can investigate the quality of commodity medicinal material and patent medicine; 4. the variation of some chemical composition from the traceable preparation of standard finger-print; 5. can detect between raw material and finished product, the stability of quality between finished product batch.Spice in bittern is comprised of several and even tens kinds of medicinal materials, and between complicated ingredient, also may have complicated collaborative or antagonism.Therefore, for a kind of control of quality of complex system, finger-print is not stinted for the highly effective means of one, but the application of fingerprint chromatogram in food is also considerably less, application in bittern does not also find that there is report, a kind of innovation means of food quality evaluation so it also be can yet be regarded as.
Guilin brine composition is very complicated, and its chromatographic fingerprinting has comprised complicated information, and this has also determined the diversity of its evaluation index.General in present finger-print process of establishing, what most of document was used is the similarity software for calculation of Chinese Pharmacopoeia Commission's recommendation, and what it adopted is with related coefficient similarity evaluation index as a whole; What also some people adopted is manually to calculate the evaluation index as a whole such as included angle cosine similarity and related coefficient similarity, but because of its sensitivity problem, only through such overall similarity, calculating may be the otherness between cannot complete reaction different batches finished product.And applicant calculates on the basis of Criterion finger-print at above basic overall similarity, combination degree similarity is calculated and numerical similarity parameter is evaluated finished product, to increase the sensitivity of quality assessment.The document < < similar system theory of delivering at Liu Yongsuo etc. is for the similarity evaluation [J] of chromatographic fingerprints of Chinese materia medica. chromatogram, 2005,23(2): in 158～163 > >, the special extent similarity that proposes calculates, and it has been carried out to improvement application, program similarity after improvement proves that it has higher sensitivity, more can reflect the otherness between data.No matter being that similarity software calculates, included angle cosine value is calculated or extent similarity calculates, is all to calculate for total peak part, has ignored the difference at non-total peak; Numerical similarity can better characterize the difference part at the non-total peak being left in the basket, this document < < quantitative finger print atlas of delivering people such as Shi Tao application [J] in Anshen Bunao mixture quality assessment. Chinese Pharmaceutical Journal, 2009,44(5): in the Anshen Bunao mixture quality assessment of mentioning in 386-389 > >, obtained application.Extent similarity (Q ') computing formula is Q '=1-∑ ∣ 1-X
ai/ X
bi∣/n, wherein X
airepresent a in A chromatogram
ithe peak area at peak, X
birepresent the peak area of chromatographic peak bi corresponding in B chromatogram, the number that n is chromatographic peak.Numerical similarity (Q
n) computing formula is
wherein K, L represents respectively in two chromatograms chromatographic peak number separately, n is the number at total peak.
The application be exactly the Guilin bittern that has a Guangxi characteristic be raw material, by the Guilin bittern product of taking continuous 10 different production batch, compare, adopt HPLC analytical technology to dissect the complicated quantity relative ratio relationship between composition wherein, set up its HPLC finger-print, be intended to set up a kind of scientific and effective Guilin brine quality evaluation means.
Summary of the invention
The technical problem to be solved in the present invention is to provide structure and the using method of a kind of Guilin bittern HPLC finger-print, applied corresponding method for evaluating similarity, obtain the standard finger-print of Guilin bittern, for the quality control of Guilin bittern provide a kind of rationally, the method for science.
The present invention solves the problems of the technologies described above with following technical scheme:
A construction method for Guilin bittern HPLC finger-print, comprises the steps:
(1). for the preparation of sample
Accurately take former halogen 100g and add in 500mL volumetric flask, then add 200～350mL normal butyl alcohol, shake up, after ultrasonic extraction 15～40min, shake up constant volume, after standing 3～7h, get supernatant 200mL, revolve and steam to dry, a small amount of methyl alcohol and chloroform are eluted to 10mL ampoule, and then nitrogen dries up, the Chromatographic Pure Methanol that finally adds 1～3mL fixed volume dissolves, shake up, cross 0.45 μ m membrane filtration, gained filtrate obtain for sample.
(2) .HPLC chromatographic condition
Waters e2695 high performance liquid chromatograph;
Chromatographic column: Waters XB-C
18chromatographic column (250mm × 4.6mm, 5 μ L);
Mobile phase composition is: methyl alcohol (A)-water (B), and gradient elution, methyl alcohol percent by volume is: while being 5.0%, 5-35min during 0-5min, be 5.0%～95%;
Detect wavelength: 276nm; Column temperature: 35 ℃; Flow velocity: 1.0mL/min; Sample size: 5 μ L;
(3) analyze for sample solution with this understanding, obtain the HPLC finger-print of Guilin bittern.
The Guilin bittern standard finger-print obtaining by said method, comprising 16 common characteristic fingerprint peakses, its retention time is respectively 6.975min, 7.535min, 10.841min, 12.186min, 12.517min, 12.704min, 13.051min, 14.070min, 15.287min, 16.394min, 17.732min, 21.551min, 22.724min, 24.014min, 26.510min, 30.134min.
Guilin bittern product is measured and is obtained its finger-print, by with standard finger-print comparison, extent similarity size > 0.9, numerical similarity > 0.8, as the standard that judges that whether product quality qualified.
The Guilin bittern standard finger-print and the evaluation method thereof that by technology of the present invention, make, analyzing detecting method is simple for production, and chromatographic condition is easily realized, and is applicable to control to Guilin bittern inherent quality and the foundation of quality standard; And this method precision, repeatability, stability are better, simple to operation, collection of illustrative plates characteristic peak separates better, can grasp from collection of illustrative plates global feature looks the quality condition of Guilin bittern, thereby can be used as the index of controlling Guilin brine quality.
Accompanying drawing explanation
Fig. 1 is the standard finger-print of the Guilin bittern that obtains by method of the present invention, has from left to right marked respectively No. 1, its common characteristic peak, No. 2, No. 3, No. 4,5(S in figure) number, No. 6, No. 7, No. 8, No. 9, No. 10, No. 11, No. 12, No. 13, No. 14, No. 15, No. 16.
Fig. 2 is the Guilin bittern finger-print generative process that the present invention obtains, and horizontal ordinate represents the time, and ordinate represents the liquid phase signal value at each peak.
Embodiment
The evaluation method of a set of similarity that the present invention proposes, except having adopted related coefficient similarity, has also comprised that extent similarity and numerical similarity calculate; Guilin bittern product is measured to the finger-print obtaining by method of the present invention, with standard finger-print comparison, extent similarity > 0.9, whether numerical similarity > 0.8, meet the requirements as the standard that judges that whether product quality is qualified using similarity size.
In order to guarantee the steady quality of Guilin bittern, except technological requirement is strict control, making from brine is for the front raw-material collection producer that will seek unification, the Chinese crude drug spices of purchasing preferably accomplishes that the place of production traces to the source, regularly plucks.
The present invention, by gathering the Guilin bittern of continuous 10 different production batch, carries out HPLC analysis according to method of the present invention, by each batch of collection of illustrative plates being contrasted investigate, analyzes, and has determined its common characteristic looks peak.
Embodiment 1
1. instrument
Waters e2695 high performance liquid chromatograph, Waters diode array detecting device, Waters XB-C
18chromatographic column (250mm × 4.6mm, 5 μ L), SB-5200 ultrasonic cleaner, 0.45 μ m micropore filtering film, chromatographically pure acetonitrile, methyl alcohol is purchased from Fisher Scientific company (U.S.), and analytically pure methyl alcohol, ethanol, normal butyl alcohol, chloroform, glacial acetic acid are purchased from Guangdong Guanghua Science and Technology Co., Ltd..
2. 10 production batch of raw material Guilin bittern, numbering S
1～S
10.Wherein, the acquisition time of each batch is:
S
1-20130616、S
2-20130706、S
3-20130730、S
4-20130920、S
5-20130930、S
6-20131010、S
7-20131018、S
8-20131025、S
9-20131027、S
10-20131101。
3. method and result
(1) the extraction of Guilin brine composition
Accurately take respectively 10 batches of former halogen 100g in Guilin and add in 500mL volumetric flask, more each sample adds 300mL normal butyl alcohol, shake up, after ultrasonic extraction 30min, shake up constant volume, after standing 5h, get supernatant 200mL, revolve and steam to dry, a small amount of methyl alcohol and chloroform are eluted to 10mL ampoule, and then nitrogen dries up, finally adding the chromatographically pure methyl alcohol of 2mL dissolves, shake up, cross 0.45 μ m membrane filtration, obtain 10 for sample;
(2) high-efficient liquid phase chromatogram condition
Waters e2695 high performance liquid chromatograph (quaternary pump, automatic sampler, column oven, PDA detecting device, Empower2.0 chromatographic work station); Chromatographic column: Waters XB-C
18chromatographic column (250mm × 4.6mm, 5 μ L); Mobile phase composition is: methyl alcohol (A)-water (B), and gradient elution, A phase volume number percent is: 5.0%(0-5min), and 5.0%～95%(5-35min) detection wavelength: 276nm; Column temperature: 35 ℃; Flow velocity: 1.0mL/min; Sample size: 5 μ L.
Accurately draw 10 confession sample solutions that obtain according to above-mentioned chromatographic condition analyzing and testing, obtain the HPLC finger-print of 10 batches of Guilin bittern, as shown in Figure 2.By analysis, compare, determined wherein 16 common characteristic fingerprint peakses, its retention time is respectively 6.975min, 7.535min, 10.841min, 12.186min, 12.517min, 12.704min, 13.051min, 14.070min, 15.287min, 16.394min, 17.732min, 21.551min, 22.724min, 24.014min, 26.510min, 30.134min, these common characteristic peaks have formed the fingerprint characteristic of Guilin bittern, can be used as the standard finger-print of Guilin bittern, as shown in Figure 1.Contrast this Guilin bittern of 10 batches, the relative retention time at its total peak is consistent relatively, and RSD value is 0～0.93%, meets finger-print and sets up requirement, does not affect the contrast of sample similarity.
The < < similarity evaluation 2004A version > > software that has used Chinese Pharmacopoeia Commission to recommend in the bittern finger-print process of establishing of Guilin, through this software, calculate, the related coefficient similarity of 10 batches of Guilin bittern is between 0.981～0.994, illustrate that similarity is better, brine quality good stability.And the Guilin bittern finger-print of each batch and the standard finger-print comparative analysis of generation, and after improved extent similarity and numerical similarity calculating, extent similarity is between 0.936～0.975, numerical similarity is between 0.818～0.875.Therefore, use the method control Guilin bittern product quality, extent similarity result of calculation should > 0.93, and numerical similarity calculates should > 0.8.
Using retention time with retain more stable the 5th the total chromatographic peak of peak area as reference peak, calculate relative retention time and the relative peak area at each total peak, carry out precision, reappearance and study on the stability test.
Methodological study
Precision: the Guilin bittern finished product of getting same production batch is prepared according to the method described above for sample, under above-mentioned chromatographic condition, detect finger-print, continuous sample introduction 5 times, utilize < < similarity evaluation 2004A version > > software and RSD analysis software to calculate similarity and the relative retention time of each total fingerprint peaks, relatively retain the RSD(% of peak area) value, as criterion, investigate the precision of sample, analysis result shows: similarity is almost close to 0.999, the relative retention time RSD value that calculates each chromatographic peak is 0.00%～0.53%, the relative peak area RSD value of each chromatographic peak is 0.37%～3.21%, result shows that precision is good, meet finger-print and set up requirement.
Reappearance: the Guilin bittern finished product of getting same production batch is prepared according to the method described above for sample, under above-mentioned chromatographic condition, detect finger-print, continuous sample introduction 5 times, utilize < < similarity evaluation 2004A version > > software and RSD analysis software to calculate similarity and the relative retention time of each total fingerprint peaks, relatively retain the RSD(% of peak area) value, as criterion, investigate the reappearance of sample, analysis result shows: similarity is 0.973～0.993, the relative retention time RSD value that calculates each chromatographic peak is 0.00%～0.34%, the relative peak area RSD value of each chromatographic peak is 0.72%～4.84%, result shows that reappearance is good, meet finger-print and set up requirement.
Stability: get same batch of Guilin bittern finished product and prepare according to the method described above for sample, under above-mentioned chromatographic condition, detect finger-print, 0, 4, 10, 16, 24h different time points sample introduction is measured, utilize < < similarity evaluation 2004A version > > software and RSD analysis software to calculate similarity and the relative retention time of each total fingerprint peaks, relatively retain the RSD(% of peak area) value, as criterion, investigate the stability of sample, analysis result shows: similarity is 0.987～1.000, the relative retention time RSD value that calculates each chromatographic peak is 0.00%～0.12%, the relative peak area RSD value of each chromatographic peak is 0.43%～2.94%, result shows that sample is stable in 24h, meet finger-print and set up requirement.
Embodiment 2
In the confession preparation process of sample, accurately take former halogen 100g and add in 500mL volumetric flask, then add 200mL normal butyl alcohol, shake up, after ultrasonic extraction 15min, shake up constant volume, after standing 3h, get supernatant 200mL, revolve and steam to dry, a small amount of methyl alcohol and chloroform are eluted to 10mL ampoule, and then nitrogen dries up, and the Chromatographic Pure Methanol that finally adds 1mL fixed volume dissolves.All the other operate with embodiment 1.
Embodiment 3
In the confession preparation process of sample, accurately take former halogen 100g and add in 500mL volumetric flask, then add 350mL normal butyl alcohol, shake up, after ultrasonic extraction 40min, shake up constant volume, after standing 7h, get supernatant 200mL, revolve and steam to dry, a small amount of methyl alcohol and chloroform are eluted to 10mL ampoule, and then nitrogen dries up, and the Chromatographic Pure Methanol that finally adds 3mL fixed volume dissolves.All the other operate with embodiment 1.
Claims (3)
1. a construction method for Guilin bittern HPLC finger-print, the method for employing similarity evaluation, is characterized in that comprising the steps:
(1). for the preparation of sample
Accurately take former halogen 100g and add in 500mL volumetric flask, then add 200～350mL normal butyl alcohol, shake up, after ultrasonic extraction 15～40min, shake up, constant volume, after standing 3～7h, get supernatant 200mL, revolve and steam to dry, a small amount of methyl alcohol and chloroform are eluted to 10mL ampoule, and then nitrogen dries up, the Chromatographic Pure Methanol that finally adds 1～3mL fixed volume dissolves, shake up, cross 0.45 μ m membrane filtration, gained filtrate is for sample;
(2) .HPLC chromatographic condition
Waters e2695 high performance liquid chromatograph;
Chromatographic column: Waters XB-C
18chromatographic column 250mm × 4.6mm, 5 μ L;
Mobile phase composition is: methanol-water, and gradient elution, methyl alcohol percent by volume is: while being 5.0%, 5-35min during 0-5min, be 5.0%～95%;
Detect wavelength: 276nm; Column temperature: 35 ℃; Flow velocity: 1.0mL/min; Sample size: 5 μ L;
(3) analyze for sample solution under these conditions, obtained the HPLC finger-print of Guilin bittern.
2. the construction method of Guilin as claimed in claim 1 bittern HPLC finger-print, the structure that it is characterized in that standard finger-print compares analysis by the finger-print that adopts said method to set up to 10 different production batch Guilin bittern, wherein 16 common characteristic fingerprint peakses have been determined, its retention time is respectively 6.975min, 7.535min, 10.841min, 12.186min, 12.517min, 12.704min, 13.051min, 14.070min, 15.287min, 16.394min, 17.732min, 21.551min, 22.724min, 24.014min, 26.510min, 30.134min, these common characteristic peaks have formed the fingerprint characteristic of Guilin bittern, as the standard finger-print of Guilin bittern.
3. the using method of Guilin as claimed in claim 1 or 2 bittern HPLC finger-print, it is characterized in that this cover method for evaluating similarity has comprised that extent similarity and numerical similarity calculate, Guilin bittern product is measured and obtained its finger-print, by with standard finger-print comparison, extent similarity size > 0.9, numerical similarity > 0.8, as the standard that judges qualified product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051417A (en) * | 2017-12-15 | 2018-05-18 | 湖南科技大学 | A kind of fluorescent inspection method of edible areca-nut brine |
| CN109603196A (en) * | 2018-12-25 | 2019-04-12 | 云南民族大学 | A method of the directional separation target compound from plant |
| CN116485265A (en) * | 2023-04-26 | 2023-07-25 | 青海省第三地质勘查院 | Open laboratory management system containing quality control analysis of salt lake samples |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101144992B1 (en) * | 2011-07-28 | 2012-06-27 | 대한민국 | Detecting method of garlic in mixed seasoning |
-
2014
- 2014-01-24 CN CN201410033573.4A patent/CN103743842A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101144992B1 (en) * | 2011-07-28 | 2012-06-27 | 대한민국 | Detecting method of garlic in mixed seasoning |
Non-Patent Citations (3)
| Title |
|---|
| 安莹 等: "万通酱油HPLC指纹图谱的研究及其在真伪鉴别中的应用", 《中国调味品》, vol. 36, no. 1, 31 December 2011 (2011-12-31) * |
| 张敏 等: "八角茴香水溶性成分HPLC指纹图谱及莽草酸的定量研究", 《上海中医药杂志》, vol. 45, no. 12, 31 December 2011 (2011-12-31) * |
| 曲国福 等: "香料指纹图谱及其在烟用香精质量控制中的应用概述", 《烟草科技》, no. 5, 31 December 2006 (2006-12-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051417A (en) * | 2017-12-15 | 2018-05-18 | 湖南科技大学 | A kind of fluorescent inspection method of edible areca-nut brine |
| CN108051417B (en) * | 2017-12-15 | 2020-09-29 | 湖南科技大学 | Fluorescence inspection method of edible areca-nut brine |
| CN109603196A (en) * | 2018-12-25 | 2019-04-12 | 云南民族大学 | A method of the directional separation target compound from plant |
| CN116485265A (en) * | 2023-04-26 | 2023-07-25 | 青海省第三地质勘查院 | Open laboratory management system containing quality control analysis of salt lake samples |
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Application publication date: 20140423 |