CN102759595A - Method for constructing HPLC (high performance liquid chromatography) fingerprint spectrum of chilli powder - Google Patents
Method for constructing HPLC (high performance liquid chromatography) fingerprint spectrum of chilli powder Download PDFInfo
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- CN102759595A CN102759595A CN 201210260468 CN201210260468A CN102759595A CN 102759595 A CN102759595 A CN 102759595A CN 201210260468 CN201210260468 CN 201210260468 CN 201210260468 A CN201210260468 A CN 201210260468A CN 102759595 A CN102759595 A CN 102759595A
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Abstract
The invention relates to a method for constructing an HPLC(high performance liquid chromatography) fingerprint spectrum of chilli powders, comprising the following steps: (1) preparing a sample solution, i.e. weighing 5g of chilli powders in a 50mL of test tube with a plug; adding 25mL of methanol and tetrahydrofuran mixing liquid, and evenly shaking up the plugged tube; carrying out ultrasonic extraction under water temperature of 60 DEG C; filtering with a filter paper, and collecting filtrate; subsequently adding 25mL of methanol and tetrahydrofuran mixing liquid, and carrying out ultrasonic extraction under water temperature of 60 DEG C for 10 minutes; filtering with a filter paper and then collecting filtrate, blending two filtrates, and concentrating the filtrate to 20mL at 70 DEG C using a rotary evaporator; then adding methanol and tetrahydrofuran mixture till the mixed solution reaches 50mL; and filtering by using a 0.2mu m microporous filtering film and carrying out chromatographic analysis to obtain the fingerprint spectrum of the chili powder. The standard fingerprint spectrum of the chilli powder prepared by the invention is applied to distinguishing and control of chilli powder quality; moreover, the analysis detection method of the chilli powder is conveniently carried out, the chromatogram conditions are easily implemented, and the stability and repeatability of the method are good.
Description
Technical field
The present invention relates to a kind of construction method of flavouring finger-print, particularly a kind of construction method of chilli powder HPLC finger-print.
Background technology
Chilli powder is redness or reddish yellow, and is glossy and uniform powder is by the fine ground potpourri that forms of pimiento, yellow capsicum, chilli seed and part capsicum bar, has the intrinsic peppery fragrance of capsicum.Chilli powder is one of raw material commonly used during essence is produced, and its quality control is one of index of essence product stability.Finger-print can reflect kind, quantity and the information such as ratio each other of the contained chemical constitution of chilli powder more all sidedly, and then characterizes its inherent quality effectively.Present patent application is intended to set up the chilli powder fingerprint map analyzing detection method of a cover based on the HPLC data, for the quality control of chilli powder provides scientific basis and guidance.
Summary of the invention
The purpose of this invention is to provide a kind of construction method of chilli powder HPLC finger-print and the resulting chilli powder standard finger-print of method thus, is that the quality control of chilli powder provides scientific basis and guidance through this standard finger-print.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of construction method of chilli powder HPLC finger-print comprises the steps:
1), the preparation of need testing solution
Take by weighing 5g chilli powder in the 50mL test tube with ground stopper; Add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), jump a queue shake up after, under 60 ℃ of water temperatures, carry out Extraction by Ultrasound 20min; With collecting filtrating behind the filter paper filtering; (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), ultrasonic Extraction 10min under 60 ℃ of water temperatures is with collecting filtrating behind the filter paper filtering to add 25mL methyl alcohol and tetrahydrofuran mixed liquor again; Merge filtrating twice; Be concentrated into 20mL with rotary evaporator at 70 ℃, then use methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) be settled to 50mL, through the laggard circumstances in which people get things ready for a trip analysis of spectrum of 0.2 μ m filtering with microporous membrane.
2), high-efficient liquid phase chromatogram condition
Agilent 1200 type high performance liquid chromatographs (quaternary pump, online degasser, automatic sampler, column oven, DAD detecting device and ChemStation chromatographic work station)
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 * 150mm, 5 μ m)
Moving phase consists of methyl alcohol: water=65:35 (volume ratio), flow velocity 1.0mL/min, 30 ℃ of column temperatures, DAD scanning wavelength 280nm, reference wavelength 360nm, sample size 10 μ L.
Analyze need testing solution with this understanding, obtain the finger-print of chilli powder.
A kind of chilli powder standard finger-print that obtains by above-mentioned said construction method; This standard finger-print compares through 10 batches of chilli powders being adopted the analysis of the finger-print of said method foundation; Confirmed 2 common characteristic peaks, its retention time is respectively 9.886min, 15.219min; These common characteristic peaks have constituted the fingerprint characteristic of chilli powder, can be used as the standard finger-print of chilli powder.
A kind of analyzing detecting method of chilli powder HPLC finger-print comprises the steps:
1), the extraction of chilli powder composition
Take by weighing 5g chilli powder in the 50mL test tube with ground stopper, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), jump a queue shake up after; Under 60 ℃ of water temperatures, carry out Extraction by Ultrasound 20min,, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) again with collecting filtrating behind the filter paper filtering; Ultrasonic Extraction 10min under 60 ℃ of water temperatures; With collecting filtrating behind the filter paper filtering, merge filtrating twice, be concentrated into 20mL with rotary evaporator at 70 ℃; Then use methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) be settled to 50mL; Behind 0.2 μ m filtering with microporous membrane, be liquid to be measured, carry out stratographic analysis.
2), high-efficient liquid phase chromatogram condition
Agilent 1200 type high performance liquid chromatographs (quaternary pump, online degasser, automatic sampler, column oven, DAD detecting device and ChemStation chromatographic work station)
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 * 150mm, 5 μ m)
Moving phase consists of methyl alcohol: water=65: 35 (volume ratio), flow velocity 1.0mL/min, 30 ℃ of column temperatures, DAD scanning wavelength 280nm, reference wavelength 360nm, sample size 10 μ L.
Analytical procedure 1 with this understanding) liquid to be measured that makes, obtain the finger-print of chilli powder, and analyze comparison with the above-mentioned chilli powder standard finger-print that obtains.
Advantage that the present invention had and beneficial effect are:
The chilli powder standard finger-print that the present invention makes is applicable to discriminating and the control to the chilli powder quality, and the analyzing detecting method of chilli powder is simple for production, and chromatographic condition realizes that easily the stability of method and reappearance are all relatively good.
Description of drawings
Fig. 1 is the HPLC chromatogram of a certain chilli powder sample;
Fig. 2 is a standard capsicim class material chromatogram;
The standard finger-print of the chilli powder that Fig. 3 obtains for the present invention has from left to right marked No. 1, its common characteristic peak, No. 2 respectively among the figure, through with the comparison of standard capsicim class material, No. 1 peak is a capsicim, No. 2 peaks are Dihydrocapsaicin.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but does not limit protection scope of the present invention.
Embodiment 1
A kind of construction method of chilli powder HPLC finger-print comprises the steps:
1), the preparation of need testing solution
Take by weighing 5g chilli powder in the 50mL test tube with ground stopper, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), jump a queue shake up after; Under 60 ℃ of water temperatures, carry out Extraction by Ultrasound 20min,, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) again with collecting filtrating behind the filter paper filtering; Ultrasonic Extraction 10min under 60 ℃ of water temperatures; With collecting filtrating behind the filter paper filtering, merge filtrating twice, be concentrated into 20mL with rotary evaporator at 70 ℃; Then use methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) be settled to 50mL; Behind 0.2 μ m filtering with microporous membrane, get need testing solution, carry out stratographic analysis.
2), high-efficient liquid phase chromatogram condition
Agilent 1200 type high performance liquid chromatographs (quaternary pump, online degasser, automatic sampler, column oven, DAD detecting device and ChemStation chromatographic work station)
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 * 150mm, 5 μ m)
Moving phase consists of methyl alcohol: water=65: 35 (volume ratio), flow velocity 1.0mL/min, 30 ℃ of column temperatures, DAD scanning wavelength 280nm, reference wavelength 360nm, sample size 10 μ L.
Analyze need testing solution with this understanding, obtain the finger-print of chilli powder.
With this understanding, analyze a certain chilli powder sample, get the HPLC chromatogram, as shown in Figure 1.
According to the method described above 10 batches of chilli powders are set up finger-print, the record chromatogram has been confirmed 2 common characteristic peaks; Its retention time is respectively 9.886min, 15.219min, and these common characteristic peaks have constituted the fingerprint characteristic of chilli powder; Can be used as the standard finger-print of chilli powder; As shown in Figure 3, and through knowing with the contrast of Fig. 2 standard capsicim class material chromatogram: No. 1 peak is a capsicim, and No. 2 peaks are Dihydrocapsaicin.
Wherein the chromatographic peak degree of separation with No. 2 peaks is good, intensity is high, and is the total peak of all batches figure, therefore is chosen as the object of reference peak, and is carrying out selecting for use the data at No. 2 peaks to calculate when stability and precision are investigated test.
Methodological study
Stability test: get same confession examination solution, respectively 0,3,6,9,12,15,18,21, the 24h different time points detects finger-print, again with the RSD value of included angle cosine similarity calculation sample and 0h sample similarity.Stability with assess sample and instrument.The result shows: similarity RSD value is 3.8%.Explain that confession examination solution and testing tool are basicly stable in 24h, do not have significant change, meet the requirement that finger-print detects.
Precision test: get same confession examination solution; Continuous sample introduction 6 times utilizes the included angle cosine similarity to calculate, and the collection of illustrative plates of back 5 sample introductions is carried out similarity with the 1st sample introduction collection of illustrative plates respectively calculate; Draw the RSD value of back 5 sample similarities, in order to estimate the precision of this method.The result shows: its similarity RSD value is 2.6%.The overall precision of illustrative experiment is good, meets the requirement that finger-print detects.
Claims (3)
1. the construction method of a chilli powder HPLC finger-print is characterized in that: comprise the steps:
1), the preparation of need testing solution
Take by weighing 5g chilli powder in the 50mL test tube with ground stopper; Add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), jump a queue shake up after, under 60 ℃ of water temperatures, carry out Extraction by Ultrasound 20min; With collecting filtrating behind the filter paper filtering; (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), ultrasonic Extraction 10min under 60 ℃ of water temperatures is with collecting filtrating behind the filter paper filtering to add 25mL methyl alcohol and tetrahydrofuran mixed liquor again; Merge filtrating twice; Be concentrated into 20mL with rotary evaporator at 70 ℃, then use methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) be settled to 50mL, through the laggard circumstances in which people get things ready for a trip analysis of spectrum of 0.2 μ m filtering with microporous membrane;
2), high-efficient liquid phase chromatogram condition
Agilent 1200 type high performance liquid chromatographs
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 * 150mm, 5 μ m)
Moving phase consists of methyl alcohol: water=65: 35 (volume ratio), flow velocity 1.0mL/min, 30 ℃ of column temperatures, DAD scanning wavelength 280nm, reference wavelength 360nm, sample size 10 μ L;
Analyze need testing solution with this understanding, obtain the finger-print of chilli powder.
2. chilli powder standard finger-print that obtains by above-mentioned said construction method; It is characterized in that: this standard finger-print compares through 10 batches of chilli powders being adopted the analysis of the finger-print of said method foundation; Confirmed 2 common characteristic peaks, its retention time is respectively 9.886min, 15.219min; These common characteristic peaks have constituted the fingerprint characteristic of chilli powder, can be used as the standard finger-print of chilli powder.
3. the analyzing detecting method of a chilli powder HPLC finger-print is characterized in that: comprise the steps:
1), the extraction of chilli powder composition
Take by weighing 5g chilli powder in the 50mL test tube with ground stopper, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)), jump a queue shake up after; Under 60 ℃ of water temperatures, carry out Extraction by Ultrasound 20min,, add 25mL methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) again with collecting filtrating behind the filter paper filtering; Ultrasonic Extraction 10min under 60 ℃ of water temperatures; With collecting filtrating behind the filter paper filtering, merge filtrating twice, be concentrated into 20mL with rotary evaporator at 70 ℃; Then use methyl alcohol and tetrahydrofuran mixed liquor (methyl alcohol: tetrahydrofuran=1: 1 (volume ratio)) be settled to 50mL; Behind 0.2 μ m filtering with microporous membrane, be liquid to be measured, carry out stratographic analysis;
2), high-efficient liquid phase chromatogram condition
Agilent 1200 type high performance liquid chromatographs
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 * 150mm, 5 μ m)
Moving phase consists of methyl alcohol: water=65: 35 (volume ratio), flow velocity 1.0mL/min, 30 ℃ of column temperatures, DAD scanning wavelength 280nm, reference wavelength 360nm, sample size 10 μ L;
Analytical procedure 1 with this understanding) liquid to be measured that makes, obtain the finger-print of chilli powder, and analyze comparison with the chilli powder standard finger-print that claim 2 obtains.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546669A (en) * | 2016-10-14 | 2017-03-29 | 浙江鼎泰药业股份有限公司 | The detection method of capsaicin content in emplastrum |
| CN110441425A (en) * | 2019-08-09 | 2019-11-12 | 深圳市赛泰诺生物技术有限公司 | A kind of capsaicine detection method |
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2012
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546669A (en) * | 2016-10-14 | 2017-03-29 | 浙江鼎泰药业股份有限公司 | The detection method of capsaicin content in emplastrum |
| CN110441425A (en) * | 2019-08-09 | 2019-11-12 | 深圳市赛泰诺生物技术有限公司 | A kind of capsaicine detection method |
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Application publication date: 20121031 |