CN103472145A - Method for analyzing volatile components of lemon essential oil - Google Patents

Abstract

The invention relates to a method for analyzing the volatile components of lemon essential oil. The method comprises the following steps: putting 10 g of lemon sample and 50 ml of deionized water to a round-bottom flask with the volume of 250 ml; adding zeolites to the round-bottom flask; connecting the round-bottom flask to a distillation-extraction device; heating the round-bottom flask through a heating jacket and keeping the mixture in a micro-boiling state; adding 50 ml of redistilled anhydrous diethyl ether to a solvent bottle; keeping the redistilled anhydrous ether in a micro-boiling state through water bath; filling condensed water into the distillation-extraction device; performing continuous extraction for 4 h; after the extraction, taking the solvent bottle down; performing rotary evaporation on the solution in the solvent bottle in a water bath of 40 DEG C, so as to remove most diethyl ether; concentrating the solution in the solvent bottle until the volume of the solution is about 1 ml; adding anhydrous sodium sulfate to the concentrated solution to drying the concentrated solution; obtaining 0.2 Mul of sample after filtration; performing GC-MS analysis and identification on the sample. According to the method, distillation and extraction are combined. The extraction time is relatively long, so that the most kinds of compounds are obtained, and the flavor profile of the sample can be reflected compressively.

Description

A kind of analytical approach of lemon volatile ingredient

Technical field

The present invention relates to a kind of distillation extraction simultaneously that uses and measure the method for lemon volatile ingredient in conjunction with the GC-MS coupling technique.

Background technology

Lemon (1emon) claims again lemon fruit, lemon, the female fruit of benefit etc.Lemon branch, leaf, flower, fruit all contain special aromatic oil---lemon.Lemon is the quality raw materials of producing food, commodity essence and flavoring agent, and the ability of regulating neuron nocuity and pain reaction is arranged.At present, the extraction of essential oil is a lot of with the technology of separating.But the lemon composition is analyzed relatively less, setting up component analyzing method, that later exploration is set up to the lemon etalon is significant, and being intended to provides reference for the exploitation of lemon.

Summary of the invention

The analytical approach that the purpose of this invention is to provide a kind of lemon volatile ingredient.

The technical solution used in the present invention is:

A kind of analytical approach of lemon volatile ingredient, comprise the steps:

Get 10g lemon sample and 50ml deionized water in the 250ml round-bottomed flask, add zeolite, be connected to distilling and extracting device simultaneously, use the heating jacket heating to keep slight boiling condition; In solvent bottle, add 50ml heavily to steam absolute ether, water-bath keeps micro-boiling; The condensate water of distilling and extracting device access simultaneously, continuous extraction 4h, after extraction finishes, take off solvent bottle, 40 ℃ of water-bath rotary evaporations, remove most of ether solvent, be concentrated into 1ml left and right solution, add anhydrous sodium sulfate drying, filter laggard 0.2 μ l sample to the GC-MS Analysis and Identification.

Preferably, described GC-MS Analysis and Identification condition is:

GC condition: chromatographic column HP-5MS elastic capillary-column (60m * 0.25 μ m * 0.25mm): carrier gas: He gas, flow: lmL/min, sample size is 0.2 μ L, shunt mode, split ratio is 50:1, injector temperature: 250 ℃.Solvent delay 2min; Heating schedule: 40 ℃ of initial temperatures, keep 2min, rise to 180 ℃ with 3 ℃/min, keep 10min, rise to 250 ℃ with 10 ℃/min, keep 20min.

Mass spectrum condition: ionization mode: 230 ℃ of EI ion source temperatures, electron energy 70eV, mass scanning scope: 33m/z～450m/z.Adopting scan mode is the full scan pattern.

The beneficial effect that the present invention has:

The present invention's distillation extraction simultaneously realizes by while heated sample liquid phase and organic solvent to boiling, in the time of distillation and extraction, only needs a small amount of solvent just can extract a large amount of samples, and fragrance component is concentrated.Integrate distillation and extraction, because extraction time is longer, the classes of compounds obtained is maximum, can reflect more all sidedly sample local flavor profile.

The accompanying drawing explanation

Fig. 1 is that lemon of the present invention is analyzed the total ion current spectrogram obtained through GC-MS.

Embodiment

Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.

Embodiment 1

A kind of analytical approach of lemon volatile ingredient, comprise the steps:

Get 10g lemon sample and 50ml deionized water in the 250ml round-bottomed flask, add zeolite, be connected to distilling and extracting device simultaneously, use the heating jacket heating to keep slight boiling condition; In solvent bottle, add 50ml heavily to steam absolute ether, water-bath keeps micro-boiling; The condensate water of distilling and extracting device access simultaneously, continuous extraction 4h, after extraction finishes, take off solvent bottle, 40 ℃ of water-bath rotary evaporations, remove most of ether solvent, be concentrated into 1ml left and right solution, add anhydrous sodium sulfate drying, filter laggard 0.2 μ l sample to the GC-MS Analysis and Identification;

Described GC-MS Analysis and Identification condition is:

GC condition: chromatographic column HP-5MS elastic capillary-column (60m * 0.25 μ m * 0.25mm): carrier gas: He gas, flow: lmL/min, sample size is 0.2 μ L, shunt mode, split ratio is 50:1, injector temperature: 250 ℃.Solvent delay 2min;

Heating schedule: 40 ℃ of initial temperatures, keep 2min, rise to 180 ℃ with 3 ℃/min, keep 10min, rise to 250 ℃ with 10 ℃/min, keep 20min.

Mass spectrum condition: ionization mode: 230 ℃ of EI ion source temperatures, electron energy 70eV, mass scanning scope: 33m/z～450m/z.Adopting scan mode is the full scan pattern.

Adopt GC-MS to carry out qualitative and quantitative analysis to the essential oil extracted, obtain lemon total ion current spectrogram (as shown in Figure 1), detect 84 cutting edges of a knife or a sword, identify the relative mass mark in the kind more than 50 of the compound more than 0.1, with alkene class and alcohol compound (as shown in table 1) in the majority.

Table 1

Lemon GC-MS analysis result

Claims (2)

1. the analytical approach of a lemon volatile ingredient, it is characterized in that: comprise the steps: to get 10g lemon sample and 50ml deionized water in the 250ml round-bottomed flask, add zeolite, be connected to distilling and extracting device simultaneously, use the heating jacket heating to keep slight boiling condition; In solvent bottle, add 50ml heavily to steam absolute ether, water-bath keeps micro-boiling; The condensate water of distilling and extracting device access simultaneously, continuous extraction 4h, after extraction finishes, take off solvent bottle, 40 ℃ of water-bath rotary evaporations, remove most of ether solvent, be concentrated into 1ml left and right solution, add anhydrous sodium sulfate drying, filter laggard 0.2 μ l sample to the GC-MS Analysis and Identification.

2. a kind of analytical approach of lemon volatile ingredient according to claim 1, it is characterized in that: described GC-MS Analysis and Identification condition is: the GC condition: chromatographic column HP-5MS elastic capillary-column (60m * 0.25 μ m * 0.25mm): carrier gas: He gas, flow: lmL/min, sample size is 0.2 μ L, shunt mode, split ratio is 50:1, injector temperature: 250 ℃.Solvent delay 2min.Heating schedule: 40 ℃ of initial temperatures, keep 2min, rise to 180 ℃ with 3 ℃/min, keep 10min, rise to 250 ℃ with 10 ℃/min, keep 20min.

Mass spectrum condition: ionization mode: 230 ℃ of EI ion source temperatures, electron energy 70eV, mass scanning scope: 33m/z～450m/z.Adopting scan mode is the full scan pattern.

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