CN109580841A - A kind of solid phase microextraction detects the detection method of essential oil content in rose product - Google Patents
A kind of solid phase microextraction detects the detection method of essential oil content in rose product Download PDFInfo
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Abstract
The present invention relates to Rosa Damascana detection technique field, in particular to the detection method of essential oil content in a kind of solid phase microextraction detection rose product, can the content quickly and easily to essential oil in rose detect.Technical points include S1: preparing internal standard solution；S2: sample pretreatment carries out water to sample and raises Aqueous extracts, extracts to Aqueous extracts, internal standard solution is added in extraction process into Aqueous extracts；S3: pretreated sample is subjected to Spectrometry；S4: according to Spectrometry as a result, and combine internal standard solution concentration calculation rose wate extract in citronellol, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L；S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated；Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose‑3÷0.92。
Description
Technical field
The invention belongs to Rosa Damascana detection technique field, in particular in a kind of solid phase microextraction detection rose product
The detection method of essential oil content.
Background technique
Rose (Rosa rugosa) is rosaceae, rose, and flower-shape beauty is fresh, fragrance is strong, have it is edible,
The multiple uses such as medicinal, health care, beauty, ornamental, are one of one of big famous flower in China ten and the four cut-flowers in the world.Rhodamine toner
Oil is the hat of fresh flower oil, includes a variety of effective fragrance ingredients, and as traditional beauty product, having improves skin quality, desalinates black
Effect of element；Uterus is nourished in more adjustable endocrine, alleviates dysmenorrhea.Rosa Damascana fragrant is even more as traditional fragrance
The essential fragrant body note material of women.Research shows that Rosa Damascana also has the function of antibacterial bacteriostatic, and to Escherichia coli, golden yellow Portugal
Grape coccus, salmonella typhimurium is more sensitive and has angst resistance effect, has huge Development volue.
Notification number is that the Chinese invention patent of CN103063632B discloses a kind of method for detecting Essential Oil from Oil-Bearing Rose,
It is handled rose using materials such as liquid nitrogen, dimethyl sulfoxides, flows out essential oil, recycles fluorescent staining etc. later
Reason mode handles sample.The detection method, it is cumbersome, and the dangerous material such as liquid nitrogen, dimethyl sulfoxide are used, implement
It is more difficult.
Summary of the invention
The object of the present invention is to provide a kind of solid phase microextraction detection rose product in essential oil content detection method,
Can the content quickly and easily to essential oil in rose detect.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of solid phase microextraction detects the detection method of essential oil content in rose product, comprising the following steps:
S1: internal standard solution is prepared；
S2: sample pretreatment, to sample carry out water raise Aqueous extracts, Aqueous extracts are extracted, in extraction process to
Internal standard solution is added in Aqueous extracts；
S3: pretreated rose wate extract is subjected to Spectrometry；
S4: according to Spectrometry as a result, and combine internal standard solution concentration calculation rose wate extract in citronellol,
Bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L；
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated；Meter
Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
Further, increase S6 behind S5, the phase of essential oil total amount in rose wate extract is calculated according to calculated N value
To concentration W, ‰；W=N ÷ 629180 × 1000.
Further, in S1 step, internal standard solution is 2- nonyl alcohol solution.
Further, in S2 step, sample pretreatment process is that sample is added in ml headspace bottle, and sodium chloride and internal standard is added
Liquid, sealing, magnetic agitation；It is inserted into extracting head, extracts under water bath condition, is analyzed later.
Further, in S3 step, chromatographic condition is capillary chromatographic column: 30m × 0.25mm × 0.50 μm WAXETR；
Column temperature program: 50 DEG C of initial temperature, constant temperature 2min, 80 DEG C are warming up to 3 DEG C/min, 115 DEG C are warming up to 10 DEG C/min, with 3
DEG C/min is warming up to 240 DEG C, keep 5min；Carrier gas, high-purity helium: purity >=99.999%；Flow velocity: 1mL/min is not diverted into
Sample；Injector temperature: 230 DEG C.
Further, in S3 step, Mass Spectrometry Conditions are ion source temperature: 230 DEG C；Transmission line temperature: 240 DEG C；Electronics bangs
Hit source: 70eV；Scanning range: 29~300amu.
Further, in S2 step, when carrying out extracting operation, allyl hexanoate is added into Aqueous extracts.
Further, the volume ratio of allyl hexanoate and rose wate extract is 1:20.
Further, in S2 step, it is to extract sample in two times as in 60-70 DEG C of water-bath that water, which proposes operating process,.
Further, during water mentions, magnesium formate is added into solution.
The beneficial effects of the present invention are:
1. the method that the present invention develops can pass through four kinds of objects only by the content of four kinds of substances in detection rose
Matter calculates and shifts onto out the content of essential oil and the relative concentration of essential oil in rose, and method is simple, easy to operate, has started this
The beginning that essential oil content in rose is detected in field.
2. selecting 2- nonyl alcohol to do internal standard solution in the present invention, the molecular structure of 2- nonyl alcohol, property are similar to component to be measured, and
Appearance near component to be measured；Meanwhile this substance of 2- nonyl alcohol is free of in rose, 2- nonyl alcohol can be with each group of other in sample
Divide and is kept completely separate, it being capable of independent appearance on chromatogram；2- nonyl alcohol and sample effect of dissolving each other are preferable, and will not be with rose flower beverage
Irreversible chemical reaction occurs for this complex sample.
3. each substance separating effect is preferable in sample under this chromatography-Mass Spectrometry Conditions, obviously do not drag peak or overlapping existing
As.
4. allyl hexanoate is low pole substance, allyl hexanoate is added into rose wate extract in extraction to be changed
The polarity for becoming entire extraction system makes to extract range expansion, improves effect of extracting.
5. magnesium formate can destroy the suberin layer of the cell wall of plant eleocyte, to make the volatilization in eleocyte
Oily quickly outflow, and then water can be reduced and mention the time, save enterprise's production cost.
Specific embodiment
Below in conjunction with specific embodiment, technical solution of the present invention is clearly and completely described.Obviously, it is retouched
The embodiment stated is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, originally
Field those of ordinary skill every other embodiment obtained without making creative work, belongs to the present invention
The range of protection.
A kind of solid phase microextraction detects the detection method of essential oil content in rose product, each embodiment specific as follows.
Embodiment 1
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 70 DEG C of water-baths with 200mL moisture,
Each 1h merges Aqueous extracts twice.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution of 10 μ L, is put into magnetic force
Stirring rotator, sealing；After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in apart from sample surfaces about
The upper space of 20mm after extracting 30min under 50 DEG C of bath temperatures, takes out handle, is directly entered following detection step.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 be citronellol in detection and calculated rose product in known 20 kinds of essential oil substances, bata-phenethyl alcohol, geraniol and
Ratio shared by four kinds of substances of eugenol.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3
÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 2
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 60 DEG C of water-baths with 200mL moisture,
Each 1h merges Aqueous extracts twice.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution of 10 μ L, is put into magnetic force
Stirring rotator, sealing；After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in apart from sample surfaces about
The upper space of 20mm after extracting 30min under 50 DEG C of bath temperatures, takes out handle, is directly entered following detection step.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 3
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 70 DEG C of water-baths with 200mL moisture,
Each 1h merges Aqueous extracts twice.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution and caproic acid alkene of 10 μ L
Propyl ester liquid, wherein the volume ratio of allyl hexanoate and rose wate extract is 1:20, is put into magnetic agitation rotor, is sealed；?
After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in the upper space apart from sample surfaces about 20mm, 50
After extracting 30min under DEG C bath temperature, handle is taken out, following detection step is directly entered.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 4
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 70 DEG C of water-baths with 200mL moisture,
Each 1h merges Aqueous extracts twice.It is extracting with dissolving 2g magnesium formate in 200mL water in advance.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution of 10 μ L, is put into magnetic force
Stirring rotator, sealing；After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in apart from sample surfaces about
The upper space of 20mm after extracting 30min under 50 DEG C of bath temperatures, takes out handle, is directly entered following detection step.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 5
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 80 DEG C of water-baths with 200mL moisture,
Each 40min merges Aqueous extracts twice.It is extracting with dissolving 2g magnesium formate in 200mL water in advance.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution of 10 μ L, is put into magnetic force
Stirring rotator, sealing；After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in apart from sample surfaces about
The upper space of 20mm after extracting 30min under 50 DEG C of bath temperatures, takes out handle, is directly entered following detection step.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 6
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 80 DEG C of water-baths with 200mL moisture,
Each 1h merges Aqueous extracts twice.It is extracting with dissolving 2g magnesium formate in 200mL water in advance.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution and caproic acid alkene of 10 μ L
Propyl ester liquid, wherein the volume ratio of allyl hexanoate and rose wate extract is 1:20, is put into magnetic agitation rotor, is sealed；?
After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in the upper space apart from sample surfaces about 20mm, 50
After extracting 30min under DEG C bath temperature, handle is taken out, following detection step is directly entered.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Embodiment 7
S1: internal standard solution is prepared.100 μ L of 2- nonyl alcohol is pipetted to be configured to 100mL volumetric flask with dehydrated alcohol constant volume
823mg/L standard reserving solution.Standard reserving solution 2.5mL is pipetted into 25mL volumetric flask, with dehydrated alcohol constant volume, is configured to
82.3mg/L internal standard solution is placed at low-temperature dark and saves for use.
S2: sample pretreatment weighs the fresh rose of 25g, is extracted twice in 80 DEG C of water-baths with 200mL moisture,
Each 30min merges Aqueous extracts twice.It is extracting with dissolving 2g magnesium formate in 200mL water in advance.
Aqueous extracts 2mL is pipetted in the ml headspace bottle of 20mL, 3gNaCl is added, adds the internal standard solution and caproic acid alkene of 10 μ L
Propyl ester liquid, wherein the volume ratio of allyl hexanoate and rose wate extract is 1:20, is put into magnetic agitation rotor, is sealed；?
After stirring 1h under 750r/min revolving speed, it is inserted into extracting head, fiber head is placed in the upper space apart from sample surfaces about 20mm, 50
After extracting 30min under DEG C bath temperature, handle is taken out, following detection step is directly entered.
S3: pretreated rose wate extract is subjected to Spectrometry.Chromatographic condition is capillary chromatographic column:
WAXETR30m×0.25mm×0.50μm；Column temperature program: 50 DEG C of initial temperature, constant temperature 2min is warming up to 80 DEG C with 3 DEG C/min,
115 DEG C are warming up to 10 DEG C/min, 240 DEG C is warming up to 3 DEG C/min, keeps 5min；Carrier gas, high-purity helium: purity >=
99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injector temperature: 230 DEG C.Mass Spectrometry Conditions are ion source temperature: 230 DEG C；
Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；Scanning range: 29~300amu.
S4: according to the peak area for the various substances that Spectrometry detects, and the concentration calculation rose of internal standard solution is combined
Citronellol in rare colored Aqueous extracts, bata-phenethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L.
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated.Its
In, 0.92 is citronellol, bata-phenethyl alcohol, geraniol and the eugenol four in detection and calculated known 20 kinds of essential oil substances
Ratio shared by kind substance.Calculate essential oil material concentration R, mg/g, R=M × (200/25) × 10 in rose-3÷0.92。
S6: calculating the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, and ‰；W=N ÷
629180×1000.Wherein, known 20 kinds of active principle measured value contents in the pure essential oil of 629180mg/L system 100%.
Detection method
1. the world Ni Shi rose industry limited liability company is taken to produce nine rose beverage flower this element drinking-water honey peach tastes respectively
Plant beverage, nine rose beverage flower this element drink grapefruit taste plant beverages, nine rose-juice drinks and Kunming, Yunnan, are protected
The produced fresh rose flower juice in mountain shop carries out chromatograph mass spectrum analysis, as the result is shown citronellol, bata-phenethyl alcohol, geraniol and eugenol four
Kind substance peak area is larger, calculates separately the ratio that these four substances account for known 20 kinds of essential oil substances in each sample, final to count
Calculating average value is 0.92.
2. after pure essential oil dehydrated alcohol gradient dilution, direct injected detection, essential oil substance known to 20 kinds of measurement: australene
Alkene；Nopinene；Geranic acid methyl esters；Citronellyl acetate；α-terpineol；Citronellol；Nerol；Geraniol；Nerolidol；17
Alkane；Linalool；Bata-phenethyl alcohol；Methyl eugenol；Tricosane；Rose oxide；Linalool；Beta-myrcene；D- limonene；21
Alkane；Nonadecane.Obtaining known 20 kinds of active principle measured value contents in 100% pure essential oil according to calculated by peak area is
629180mg/L。
3.M=82.3 × 5 × 10-3× (B/A) mg/L, wherein B is citronellol, bata-phenethyl alcohol, geraniol and eugenol
The sum of four kinds of substance peak areas, A are internal standard compound peak area.
Testing result
Experimental result shows that detection of the invention and calculation method more convenient, quickly can contain essential oil in rose
Amount and concentration are detected.Compared with Example 1, each substance peak area value that chromatography-mass spectroscopy testing result is shown is equal for embodiment 3
It changes, but the concentration value M of four kinds of citronellol in final sample, bata-phenethyl alcohol, geraniol and eugenol substances does not have
Substantially change, when being pre-processed to sample, be added allyl hexanoate can facilitated extraction effect, and the improvement of effect of extracting
Illustrate that sample pretreating method of the invention can be also applicable in even for the sample of low concentration, to expand side of the invention
The use scope of method.Compared with Example 1, magnesium formate is added when water mentions in embodiment 4, the peak area of substance without significant change,
But embodiment 5 is compared with Example 4, water mentions the time and shortens, and for substance peak area also without significant change, this illustrates magnesium formate energy
Enough accelerate the release of essential oil in rose.
Claims (10)
1. the detection method of essential oil content in a kind of solid phase microextraction detection rose product, which is characterized in that including following step
It is rapid:
S1: internal standard solution is prepared；
S2: sample pretreatment carries out water to sample and raises Aqueous extracts, extracts to Aqueous extracts, Xiang Shuiti in extraction process
Internal standard solution is added in liquid；
S3: pretreated rose wate extract is subjected to Spectrometry；
S4: according to Spectrometry as a result, and citronellol, β-benzene in the concentration calculation rose wate extract of combination internal standard solution
Ethyl alcohol, four kinds of substances of geraniol and eugenol concentration be M, mg/L；
S5: according to calculated M value, essential oil material concentration N, mg/L, N=M ÷ 0.92 in rose wate extract is calculated；Calculate rose
It is rare to spend middle essential oil material concentration R, mg/g, R=M × (200/25) × 10-3÷0.92。
2. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 1
It is: increases S6 behind S5, calculates the relative concentration W of essential oil total amount in rose wate extract according to calculated N value, ‰；W
=N ÷ 629180 × 1000.
3. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 1
Be: in S1 step, internal standard solution is 2- nonyl alcohol solution.
4. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 1
Be: in S2 step, sample pretreatment process is that sample is added in ml headspace bottle, and sodium chloride and internal standard solution, sealing, magnetic force is added
Stirring；It is inserted into extracting head, extracts under water bath condition, is analyzed later.
5. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 1
Be: in S3 step, chromatographic condition is capillary chromatographic column: 30m × 0.25mm × 0.50 μm WAXETR；Column temperature program: it rises
Beginning temperature 50 C, constant temperature 2min are warming up to 80 DEG C with 3 DEG C/min, are warming up to 115 DEG C with 10 DEG C/min, are warming up to 3 DEG C/min
240 DEG C, keep 5min；Carrier gas, high-purity helium: purity >=99.999%；Flow velocity: 1mL/min, Splitless injecting samples；Injection port temperature
Degree: 230 DEG C.
6. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 1
Be: in S3 step, Mass Spectrometry Conditions are ion source temperature: 230 DEG C；Transmission line temperature: 240 DEG C；Electron bombardment ionization source: 70eV；It sweeps
Retouch range: 29~300amu.
7. -6 any solid phase microextraction detect the detection method of essential oil content in rose products according to claim 1,
It is characterized by: when carrying out extracting operation, allyl hexanoate is added into Aqueous extracts in S2 step.
8. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 7
Be: the volume ratio of allyl hexanoate and rose wate extract is 1:20.
9. -6 any solid phase microextraction detect the detection method of essential oil content in rose products according to claim 1,
It is characterized by: it is to extract sample in two times as in 60-70 DEG C of water-bath that water, which proposes operating process, in S2 step.
10. the detection method of essential oil content, feature in solid phase microextraction detection rose product according to claim 9
It is: during water mentions, magnesium formate is added into solution.
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| CN105974013A (en) * | 2016-04-29 | 2016-09-28 | 江苏耐雀生物工程技术有限公司 | Gas chromatography detection method of content of essential oil |
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| EP2233205A2 (en) * | 2009-03-24 | 2010-09-29 | Symrise GmbH & Co. KG | Flavor extracting device for isolation or analysis of volatile compounds |
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