CN104833742A - Analytical method for GC/MS fingerprint spectrum of components of lavendula officinalis essential oil - Google Patents

Abstract

The invention discloses an analytical method for a GC/MS fingerprint spectrum of components of lavendula officinalis essential oil. The analytical method is characterized by comprising the following steps: dissolving the lavendula officinalis essential oil into ethanol, setting gas chromatography conditions and mass spectrum conditions, and carrying out GC/MS analysis on the lavendula officinalis essential oil so as to obtain a GC/MS total ion chromatogram of the lavendula officinalis essential oil; preparing the lavendula officinalis essential oil from different batches of lavendula officinalis as test solutions, respectively carrying out GC/MS measurement, and recording total ion chromatograms; comparing the measured GC/MS total ion chromatograms of the lavendula officinalis of all batches so as to obtain a standard fingerprint spectrum, consisting of common characteristic peaks, of the lavendula officinalis essential oil. The analytical method is good in precision, reproducibility and stability, and an effective way is provided for the mass control of the lavendula officinalis essential oil.

Description

A kind of analytical approach of GC/MS finger-print of Lavender composition

Technical field

The present invention relates to the analysis and detection technology of Lavender, particularly, the present invention relates to a kind of GC/MS fingerprint analysis method of Lavender composition.

Background technology

Lavender (Lavendula officinalis), it is Perilla Labiatae, there is strong aromatic odor, have in delicate fragrance with sweet fragrance of a flower fragrance, lavender distillation can be obtained Lavender that is faint yellow or yellow transparent, and taste is slightly bitter, has the peculiar fragrance of lavender, having volatility, is the essence that important perfume base can be used for mediation soft drink, candy, ice cream, daily use chemicals etc.Lavender can be clearing heat and detoxicating, cleaning skin, controls oil content, freckle removing and whitening, the tender skin of anti-wrinkle, eye haustra-dsipelling livid ring around eye, also can promote that damaged tissues regenerates the skin-protecting functions such as recovery.It can purify, pacify soul, alleviate indignation and used-up sensation, make people can even-tempered and good-humouredly in the face of live.There is sedation effect to heart, hypertension can be reduced, pacify palpitaition, helpful for insomnia.

Lavender is the complex mixture of many dissimilar aromatics composition, and principal ingredient has linalool, bergamio, cineole, β-ocimenum (comprise cis and trans), acetic acid lavender ester, lavender alcohol etc.

Some are had about the report of Lavender analytical approach, such as: Zhang Jian, Cai Baoguo in prior art, Zhang Suning, Xiao Zuobing, " the GC-MS com-parison and analysis of Lavender chemical composition ", " food industry ", the fifth phase in 2007, discloses a kind of GC/MS analytical approach of Lavender; Zhang Chunling, Zhao Ji violent wind, Zhang Chaoying, Dang Junwei, Liu Yunai, " analyze the chemical composition of Yunnan lavender (Lavender) volatile oil with GC/MS ", " Henan science ", the 17th volume the 4th phase in 1999, also discloses a kind of GC/MS analytical approach of Lavender, but they all do not set up the reliable fingerprint analysis method of system to Lavender, the quality of Lavender effectively can not be controlled.

Summary of the invention

Goal of the invention: the analytical approach that the invention provides a kind of GC/MS finger-print of Lavender composition, for the quality assessment of Lavender.

Technical scheme: analytical approach provided by the invention, specifically comprises the following steps:

One. the GC/MS of Lavender chemical composition analyzes

1. precision measures essential oil 100 μ l and is dissolved in 10ml ethanol and analyzes for GC/MS;

2. arranging GC conditions: adopt DB-624 capillary column (30m × 0.32mm × 1.8 μm) to analyze, as middle polarity post, is design for analyzing volatile priority pollutant and residual solvent; Select the capillary column of 30m can obtain good separating effect also can be well controlled analysis time simultaneously.Carrier gas is high pure nitrogen; flow rate of carrier gas is 1.0mL/min; split ratio 10:1; select suitable flow rate of carrier gas to make each component in sample can both reach baseline separation under fixing analysis time to be unlikely to again to disperse very much to increase analysis time simultaneously; the split ratio of 10:1 can make sample enter chromatographic column after shunting, protective hair capillary column while guarantee analytical effect.Injector temperature 200 DEG C, detector temperature is 220 DEG C, adopt temperature programme: initial temperature 50 DEG C, keep 5.0min, 6 DEG C/min rises to 200 DEG C, keeps 1min, sample introduction 1 μ L, because containing much dissimilar aromatics in Lavender, adopt the method for temperature programme to continue to optimize condition and make them because the difference of polarity and boiling point obtains good separating effect, obtain testing result more accurately.

3. Mass Spectrometry Conditions is set: EI ion gun; Electron energy 70eV; Level Four bar temperature 150 DEG C, interface temperature 260 DEG C; Electron-multiplier voltage 1160V; Ion source temperature 230 DEG C; Employing standard mode is tuning; Select full scan pattern (SCAN), mass scan range: 40 ~ 450amu;

Two. the foundation of finger-print

1. the total ion current figure of each sample

The lavender of 8 batches of Different sources is obtained Lavender as need testing solution, carries out GC/MS mensuration respectively, record total ion current figure;

2. the foundation of standard finger-print

Contrast the GC/MS total ion current figure that the Lavenders of all batches measure, screening obtains the standard finger-print of the Lavender sample be made up of its common characteristic peak.

The invention provides a kind of standard finger-print of the cumin seed oil composition obtained by above-mentioned construction method, this standard finger-print is by adopting the com-parison and analysis of the finger-print of said method foundation to 8 batches of Lavenders, determine 9 common characteristic peaks, its retention time Rt be respectively 13.866min, 14.144min, 14.336min,

15.293min, 15.394min, 15.579min, 17.858min, 18.370min and 21.904min, these common characteristic peaks constitute the fingerprint characteristic of Lavender composition, can be used as the standard finger-print of Lavender composition.

Three, the methodological study of finger-print, is specially:

1. Precision Experiment

Get same Lavender need testing solution, continuous sample introduction 5 ~ 10 times, more each total peak-to-peak area, calculates the relative standard deviation at each peak;

2. stability experiment

Get same Lavender need testing solution, after placing 0,2,4,8,16,24h respectively, sample introduction measures, and more each total peak-to-peak area, calculates the relative standard deviation at each peak;

3. reappearance experiment

Get with a collection of Lavender 5 ~ 10 parts, prepare parallel sample solution, sample introduction, calculate the relative standard deviation of each total peak-to-peak area.

The beneficial effect of the inventive method: the precision that this method tool is good, reappearance and stability, the quality control for Lavender provides approach effectively.

Accompanying drawing explanation

Fig. 1 is the Lavender composition total ion current figure obtained by the inventive method.

Fig. 2 is the finger-print of the Lavender by the inventive method acquisition.

Embodiment:

Below in conjunction with specific embodiment, the present invention is further elaborated, but do not limit the present invention.

Embodiment

The present embodiment instrument used is: Agilent 6890-5975 gas chromatograph-mass spectrometer (GCMS), DB-624 capillary column (30m × 0.32mm × 1.8 μm), and ethanol is pure for analyzing.

The present embodiment sample used is: Lavender sample, adopts steam distillation to extract from lavender pollen obtain by the biological company limited of the resistance to sparrow in Jiangsu.

One. Lavender chemical composition GC-MS analyzes

Precision measures 100 μ l essential oils and is dissolved in 10mL ethanol and analyzes for GC/MS.

GC conditions: DB-624 capillary column (30m × 0.32mm × 1.8 μm), injector temperature 200 DEG C, detector temperature 220 DEG C, carrier gas is high pure nitrogen, and flow rate of carrier gas is 1.0mL/min, and split ratio is 10:1; Temperature programme: initial temperature 50 DEG C, keep 5.0min, 6 DEG C/min rises to 200 DEG C, keeps 1min, sample introduction 1 μ L.

Mass Spectrometry Conditions: EI ion gun; Electron energy 70eV; Level Four bar temperature 150 DEG C, interface temperature 260 DEG C; Electron-multiplier voltage 1160V; Ion source temperature 230 DEG C; Employing standard mode is tuning; Select full scan pattern, mass scan range: 40 ~ 450amu.

Two. the foundation of finger-print

1. total ion current figure:

By 8 batches of Lavender need testing solutions, each 1 μ L of each need testing solution of accurate absorption, carries out GC/MS mensuration respectively, record total ion current figure.

2. the determination at total peak:

The GC/MS total ion current figure that the Lavenders of above-mentioned all batches measure is contrasted, obtain 9 common characteristic peaks (see table 1), obtain the standard finger-print (see Fig. 2) of Lavender, they constitute the fingerprint characteristic of Lavender.

The finger-print component table of table 1 Lavender

Three. the methodological study of finger-print

1. Precision Experiment

Get same Lavender need testing solution, continuous sample introduction 6 times, more each total peak-to-peak area, calculates the relative standard deviation at each peak.Result shows, the RSD value of each total peak-to-peak area is 1.8%, is less than 3%, shows that the overall precision of testing is good, meets the requirement that finger-print detects.

2. stability experiment

Get same Lavender need testing solution, after placing 0,2,4,8,16,24h respectively, sample introduction measures, and more each total peak-to-peak area, calculates the relative standard deviation at each peak.Result shows, the RSD value of each total peak-to-peak area is 2.3%, and result is less than 3%, illustrates that need testing solution and testing tool are basicly stable in 24h, does not have significant change, meets the requirement that finger-print detects.

3. reappearance experiment

Get with a collection of Lavender 6 parts, prepare parallel sample solution, sample introduction, calculate the relative standard deviation of the peak area at each total peak.Result shows, RSD all <1.7% of each peak-to-peak area, and its value is within 3%, and the reappearance of illustrative experiment is better, meets finger-print testing requirement.

Claims (5)

1. an analytical approach for the GC/MS finger-print of Lavender composition, is characterized in that comprising the following steps:

1) Lavender is dissolved in ethanol, GC conditions is set, Mass Spectrometry Conditions is set, GC/MS analysis is carried out to Lavender, obtain the GC/MS total ion current figure of essential oil;

2) lavender of different batches is obtained Lavender as need testing solution, carry out GC/MS mensuration respectively, record total ion current figure;

3) the GC/MS total ion current figure that all batches measure is contrasted, obtain the standard finger-print of the Lavender that it is made up of common characteristic peak.

2. the analytical approach of the GC/MS finger-print of Lavender composition according to claim 1, it is characterized in that described GC conditions is: DB-624 capillary column, injector temperature 200 DEG C, detector temperature 220 DEG C, carrier gas is high pure nitrogen, flow rate of carrier gas is 1.0mL/min, temperature programme: initial temperature 50 DEG C, keeps 5.0min, 6 DEG C/min rises to 200 DEG C, keep 1min, sample introduction 1 μ L, split ratio 10:1.

3. the analytical approach of the GC/MS finger-print of Lavender composition according to claim 1, is characterized in that described Mass Spectrometry Conditions is: EI ion gun; Electron energy 70eV; Level Four bar temperature 150 DEG C, interface temperature 260 DEG C; Electron-multiplier voltage 1160V; Ion source temperature 230 DEG C; Employing standard mode is tuning; Select full scan pattern, mass scan range: 40 ~ 450amu.

4. the analytical approach of the GC-MS finger-print of Lavender composition according to claim 1, it is characterized in that, the retention time Rt at 9 total peaks that described standard finger-print has is respectively 13.866min, 14.144min, 14.336min, 15.293min, 15.394min, 15.579min, 17.858min, 18.370min and 21.904min.

5. the analytical approach of Lavender composition as claimed in claim 1, characterized by further comprising following steps:

Get same Lavender need testing solution, continuous sample introduction 5 ~ 10 times, more each total peak-to-peak area, calculates the relative standard deviation at each peak;

Get same Lavender need testing solution, after placing 0,2,4,8,16,24h respectively, sample introduction measures, and more each total peak-to-peak area, calculates the relative standard deviation at each peak;

Get with a collection of Lavender 5 ~ 10 parts, prepare parallel sample solution, sample introduction, calculate the relative standard deviation of the peak area at each total peak.