CN104391054B - The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil - Google Patents
The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil Download PDFInfo
- Publication number
- CN104391054B CN104391054B CN201410622894.8A CN201410622894A CN104391054B CN 104391054 B CN104391054 B CN 104391054B CN 201410622894 A CN201410622894 A CN 201410622894A CN 104391054 B CN104391054 B CN 104391054B
- Authority
- CN
- China
- Prior art keywords
- field
- collection
- essential oil
- ground
- illustrative plates
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
<b> the present invention relates to and Damask Rose essential oil detection technique field, field, is a kind of and field Damask Rose essential oil GC/MS fingerprint atlas detection method for standard, the present invention is using spectrogram similarity as evaluation index, from macroscopically controlling and the quality of field Damask Rose essential oil, determine the content range of its property material, fragrant comprising head, body note, bottom note, fixative ingredients and not existing standard pay close attention to body note composition, the more fully overall fragrance of control and field Damask Rose essential oil, composition and the content of high straight chain alkane are paid close attention to, effective control essential oil congealing point, chemically composition controls outward appearance and fragrance more intuitively, formulate the standard of property material quality testing on this basis, thus substantially increase accuracy of detection and detection efficiency, can be used for the quality assessment with field Damask Rose essential oil, for providing a kind of quality standard with the quality control of field Damask Rose essential oil.</b>
Description
Technical field
the present invention relates to and Damask Rose essential oil detection technique field, field, is a kind of and field Damask Rose essential oil GC/MS fingerprint atlas detection method for standard.
Background technology
rosa Damascana includes multiple effective fragrance ingredient, as traditional cosmetics, has and improves skin quality, and desalination melanin, more can regulate endocrine, nourishes uterus, relieving dysmenorrhea.Its fragrant, as traditional spices requisite fragrant body note material of women especially.Nearest research shows that Rosa Damascana has antibacterial bacteriostatic function, to Escherichia coli, staphylococcus aureus, salmonella typhimurium is comparatively responsive and have angst resistance effect (Ying Liya, Chemical Components of Rose Essential and functional study [D] thereof, Zhejiang University, 2012.), there is huge Development volue.
at present on the market with Bulgaria, as well, Pingyin, domestic Shandong, Gansu bitter water rose industry are the most outstanding for the external products such as Turkey.Rosa Damascana is a kind of secondary metabolite of rose, experiment proves that it is subject to the impact of all many condition such as growing environment and kind, constituent and content vary widely, this point just can reflect from simple physical behavior, such as Chinese bitter water rose national regulations congealing point is 10 DEG C to 15 DEG C, and Bulgarian Rosa rugosa congealing point is 16 DEG C to 23.5 DEG C; And be also clearly with the property material content that chromatogram in its standard limits, for citronellol, China's bitter water rose content is 40.0% to 54.0%, Bulgaria Damascus is 20% to 34%, Turkey Damascus is 34% to 49%, Morocco Damascus is 30% to 47%, finds out that the Rosa Damascana standard of a certain kind in a certain area can not represent and limit all Rosa Damascanas thus.The detection method of contrast " ISO9842:2003 ", it adopts polyglycol chromatographic column, its maximum operation (service) temperature is 250 DEG C, actual serviceability temperature is warmed up near 220 DEG C, the maximum boiling point material that its detection method controls is tricosane, and experiment proves and contain pentacosane in the Damask Rose essential oil of field, heptacosane and more senior alkane, their boiling point is far above 220 DEG C, direct conventional conditions measures, have constituent part cannot to detect or to go out peak imperfect, they are two years old, more serious compared with the chromatographic column column bleed of dimethyl silicone polymer by the chromatographic column column bleed of universal experience polyglycol Stationary liquid, easily there is ghost peak and not easily preserve, owing to generally calculating content many employings area normalization method, area normalization method computing formula is C
i
=A
i
/ A
always
, wherein C
i
for the content of i material, A
i
for the peak area of i material, A
always
for detect the total area, make the total area just have deviation like this, thus cause accuracy of detection to reduce, and these high boiling substances can in chromatographic system residual impurity disturb after detection, simultaneously the kind of these chain hydrocarbons and content directly affect Rosa Damascana congealing point (after testing with field Damask Rose essential oil congealing point at 24 DEG C to 29 DEG C, be different from the congealing point of other kind Rosa Damascanas in known standard), control higher aliphatic hydrocarbons all sidedly and can effectively control essential oil condensing temperature thus control its appearance character.
compare traditional chromatogram method to detect, fingerprint pattern technology emphasizes systematicness, characteristic, stability, not only the content of several property material is detected, more can reflect the characteristic of tested natural prodcuts all sidedly, but the method at present finger-print being used for Rosa Damascana detection does not also have.Can not confirm whether it is natural products at the very flourishing content just merely detecting several material today of chemical industry synthesis, for Rosa Damascana, only do the content of several property material of gas chromatographic detection, if measured object is allocated quantitatively with Prof. Du Yucang product can meet testing requirement equally, and contrast with finger-print and will find that it lacks the macroscopical feature contained by natural rose essential on the whole.
hotan as one of the ancient place of production of rose also rests on the comparatively original rose development and utilization stage, lack extraction of essential oil and product standard, well-known Xinjiang is away from ocean, belong to temperate continental climate, and Hotan Prefecture is positioned at Takla Makan Desert edge, more with temperate desert climate feature, local air oxygen detrition, precipitation is little, day and night temperature is large, Seasonal Temperature Difference is also large, light application time is long and strong, soil desertification degree is high, saline and alkaline is high, under such weather conditions and field rose shows stronger resistance thus its secondary metabolite comprises essential oil all presents local distinctive feature, its essential oil solidifying point is higher, ensure to extend perfume substantiation under dry and large temperature difference condition, the feature that the combined influence that other component contents also embody Damask Rose kind and local climate simultaneously shows, therefore existing examination criteria can not be used for defining the quality quality with field Damask Rose essential oil due to region and kind restriction.
Summary of the invention
the invention provides a kind of and field Damask Rose essential oil GC/MS fingerprint atlas detection method for standard, overcome the deficiency of above-mentioned prior art, it effectively can solve existing examination criteria due to region and kind restriction and can not be used for defining the problem with the quality quality of field Damask Rose essential oil.
technical scheme of the present invention is realized by following measures: a kind of and field Damask Rose essential oil is used for the GC/MS fingerprint atlas detection method of standard, carry out as follows: the first step, get 0.025g to 0.030g essential oil to be measured and be placed in test tube, in test tube, add normal hexane be settled to after 10mL shakes up and obtain need testing solution, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, calculates the included angle cosine value of collection of illustrative plates to be measured,
wherein: n=1 ... 133, y
i
be the peak area of the base peak of i-th corresponding retention time, x
i
for the peak area at the peak of i-th corresponding retention time in collection of illustrative plates to be measured, in collection of illustrative plates to be measured corresponding retention time without peak then peak area be 0, if the included angle cosine value of collection of illustrative plates to be measured is less than 0.9246, then essential oil to be measured is not and field Damask Rose essential oil, if included angle cosine value is greater than 0.9246, and to meet retention time in collection of illustrative plates to be measured be the content at the corresponding peak of 14.191min is 0.10% to 0.70% simultaneously, retention time is the content at the corresponding peak of 20.081min is 11.70% to 19.20%, retention time is the content at the corresponding peak of 21.167min is 1.70% to 9.00%, retention time is the content at the corresponding peak of 28.063min is 0.20% to 0.60%, retention time is the content at the corresponding peak of 29.740min is 0.20% to 0.80%, retention time is the content at the corresponding peak of 37.080min is 0.60% to 1.30%, retention time is the content at the corresponding peak of 45.931min is 19.00% to 23.00%, retention time is the content at the corresponding peak of 52.147min is 13.70% to 20.00%, retention time is the content at the corresponding peak of 63.057min is 1.30% to 3.00%, then essential oil to be measured is and field Damask Rose essential oil.
here is the further optimization and/or improvements to foregoing invention technical scheme:
the peak area of the base peak of above-mentioned corresponding retention time obtains as follows: the first step, gather No. 1 ground respectively, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, 1.5 kilograms to 2 kilograms and field Damask Rose fresh flower that No. 6 ground and the same day of No. 7 planting open, placing respectively in a reservoir with field Damask Rose fresh flower by various places after collection, then the pure water with field Damask Rose fresh flower quality 3 doubly to 4 times is added in a reservoir respectively, refluxing extraction is carried out after being heated to boiling, refluxing extraction 3h to 4h, after refluxing extraction, distillate obtains distillating phase after condenser condenses, the upper strata distillating phase is essential oil layer, the lower floor distillating phase is water layer, be separated the upper strata distillating phase and obtain No. 1 Rosa Damascana respectively, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 Rosa Damascanas, second step, get No. 1 Rosa Damascana of 0.025g to 0.030g, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 rhodamine toners are placed in test tube respectively, in test tube, then add normal hexane be respectively settled to after 10mL shakes up and obtain No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution, 3rd step, by No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution add respectively in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, No. 1 collection of illustrative plates is obtained respectively after mass spectrum, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates, 4th step, obtains the peak area of the base peak of 133 corresponding retention times after being averaged by the peak area value at peak corresponding for i-th retention time in No. 1 collection of illustrative plates, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates respectively.
in the above-mentioned first step, 8:00 to 9:30 gathers open 1.5 kilograms to 2 kilograms and the field Damask Rose fresh flower on the same day of No. 1 ground, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, No. 6 ground and No. 7 ground plantations in the morning.
above-mentioned No. 1 ground is and Tian Yetai Kyzyl village; No. 2 ground are and La Yika village, field; No. 3 ground are and Bai Shituoge clarke village, field; No. 4 ground are Hetian City; No. 5 ground are allow village with Tian Hadi; No. 6 ground are and A Rele village, field; No. 7 ground are and Ba Shi village too, field.
the column length of above-mentioned Agilent HP-5MS chromatographic column is 30m, column internal diameter is 0.25mm, thickness is 0.25 μm.
the present invention is using spectrogram similarity as evaluation index, from macroscopically controlling and the quality of field Damask Rose essential oil, determine the content range of its property material, fragrant comprising head, body note, bottom note, fixative ingredients and not existing standard pay close attention to body note composition, the more fully overall fragrance of control and field Damask Rose essential oil, composition and the content of high straight chain alkane are paid close attention to, effective control essential oil congealing point, chemically composition controls outward appearance and fragrance more intuitively, formulate the standard of property material quality testing on this basis, thus substantially increase accuracy of detection and detection efficiency, can be used for the quality assessment with field Damask Rose essential oil, for providing a kind of quality standard with the quality control of field Damask Rose essential oil.
Accompanying drawing explanation
accompanying drawing 1 is the regional finger-print that is that plant and the Rosa Damascana of field Damask Rose fresh flower extraction in the present invention and 7, field and characteristic peak stacking diagram.
Embodiment
the present invention by the restriction of following embodiment, can not determine concrete embodiment according to technical scheme of the present invention and actual conditions.
embodiment 1, be somebody's turn to do the GC/MS fingerprint atlas detection method being used for standard with field Damask Rose essential oil, carry out as follows: the first step, get 0.025g to 0.030g essential oil to be measured and be placed in test tube, in test tube, add normal hexane be settled to after 10mL shakes up and obtain need testing solution, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, calculates the included angle cosine value of collection of illustrative plates to be measured,
wherein: n=1 ... 133, y
i
be the peak area of the base peak of i-th corresponding retention time, x
i
for the peak area at the peak of i-th corresponding retention time in collection of illustrative plates to be measured, in collection of illustrative plates to be measured corresponding retention time without peak then peak area be 0, if the included angle cosine value of collection of illustrative plates to be measured is less than 0.9246, then essential oil to be measured is not and field Damask Rose essential oil, if included angle cosine value is greater than 0.9246, and to meet retention time in collection of illustrative plates to be measured be the content at the corresponding peak of 14.191min is 0.10% to 0.70% simultaneously, retention time is the content at the corresponding peak of 20.081min is 11.70% to 19.20%, retention time is the content at the corresponding peak of 21.167min is 1.70% to 9.00%, retention time is the content at the corresponding peak of 28.063min is 0.20% to 0.60%, retention time is the content at the corresponding peak of 29.740min is 0.20% to 0.80%, retention time is the content at the corresponding peak of 37.080min is 0.60% to 1.30%, retention time is the content at the corresponding peak of 45.931min is 19.00% to 23.00%, retention time is the content at the corresponding peak of 52.147min is 13.70% to 20.00%, retention time is the content at the corresponding peak of 63.057min is 1.30% to 3.00%, then essential oil to be measured is and field Damask Rose essential oil.Included angle cosine value is similarity; Cosin method is utilized to calculate similarity, it is regard spectrogram entirety as a n-dimensional vector that Cosin method calculates spectrogram similarity, represent the similarity degree of 2 spectrograms with 2 vectorial included angle cosine values, its value is between 0 to 1, and larger both the expressions of numeral are more similar.Wherein n is total peak number, the coordinate that in spectrogram, the peak area at i-th peak is tieed up as vector i-th; Such as during i=35, peak area data are 445065.9,724200.6,1721593.2,96462.0,1492129.6,1998820.1, and 2238188.4 averages are 1245209.0 is that reference is to flow control 35 dimension coordinate.Characteristic perfume material from generally acknowledged with field Damask Rose essential oil: citronellol, geraniol, linalool, the fragrance component that the content of field Damask Rose essential oil is comparatively stable: carypohyllene, β-farnesene, sagittol, affect the waxy component of essential oil congealing point: the nonadecane that content is higher, heneicosane, these nine kinds of materials of pentacosane that boiling point is higher are set about, data based on its GC/MS content, obtained component content statistics maximal value and minimum value are retained 2 decimals, as standard content scope to enter a method with the method for truncating respectively.
embodiment 2, as the optimization of above-described embodiment, in embodiment 2, the peak area of the base peak of corresponding retention time obtains as follows: the first step, gather No. 1 ground respectively, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, 1.5 kilograms to 2 kilograms and field Damask Rose fresh flower that No. 6 ground and the same day of No. 7 planting open, placing respectively in a reservoir with field Damask Rose fresh flower by various places after collection, then the pure water with field Damask Rose fresh flower quality 3 doubly to 4 times is added in a reservoir respectively, refluxing extraction is carried out after being heated to boiling, refluxing extraction 3h to 4h, after refluxing extraction, distillate obtains distillating phase after condenser condenses, the upper strata distillating phase is essential oil layer, the lower floor distillating phase is water layer, be separated the upper strata distillating phase and obtain No. 1 Rosa Damascana respectively, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 Rosa Damascanas, second step, get No. 1 Rosa Damascana of 0.025g to 0.030g, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 rhodamine toners are placed in test tube respectively, in test tube, then add normal hexane be respectively settled to after 10mL shakes up and obtain No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution, 3rd step, by No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution add respectively in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, No. 1 collection of illustrative plates is obtained respectively after mass spectrum, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates, 4th step, obtains the peak area of the base peak of 133 corresponding retention times after being averaged by the peak area value at peak corresponding for i-th retention time in No. 1 collection of illustrative plates, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates respectively.
gather the Damask Rose regional with 7, field respectively according to the method for embodiment 2 and set up finger-print analysis, determine 9 total peaks, their retention time respectively: 14.191min, 20.081min, 21.167min, 28.063min, 29.740min, 37.080min, 45.931min, 52.147min and 63.057min.Determine each component peaks area, add up each component concentration with area normalization method, determine the content range of 9 kinds of materials, determine the examination criteria based on the Damask Rose essential oil GC/MS finger-print with 7 different regions, field.With this condition collection with analyze the Rosa Damascana GC/MS finger-print of gained and above-mentioned gained finger-print and experimental result and carry out check analysis, with the peak area mean value finger-print data in contrast of the corresponding retention time of the regional Damask Rose essential oil finger-print of above-mentioned gained 7, calculate cosine similarity, should 0.9246 be greater than, and the content of 9 property materials should meet retention time is respectively 14.191min, 20.081min, 21.167min, 28.063min, 29.740min, 37.080min, 45.931min, the content range that 52.147min and 63.057min determines.
embodiment 3, as the optimization of above-described embodiment, in embodiment 3 in the first step, 8:00 to 9:30 gathers open 1.5 kilograms to 2 kilograms and the field Damask Rose fresh flower on the same day of No. 1 ground, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, No. 6 ground and No. 7 ground plantations in the morning.
embodiment 4, as the optimization of above-described embodiment, in embodiment 4, No. 1 ground is and Tian Yetai Kyzyl village; No. 2 ground are and La Yika village, field; No. 3 ground are and Bai Shituoge clarke village, field; No. 4 ground are Hetian City; No. 5 ground are allow village with Tian Hadi; No. 6 ground are and A Rele village, field; No. 7 ground are and Ba Shi village too, field.
embodiment 5, as the optimization of above-described embodiment, in embodiment 5, the column length of Agilent HP-5MS chromatographic column is 30m, column internal diameter is 0.25mm, thickness is 0.25 μm.
accompanying drawing 1 is the regional finger-print that is that plant and the Rosa Damascana of field Damask Rose fresh flower extraction in the present invention and 7, field and characteristic peak stacking diagram; Table 1 is the retention time corresponding with 9 base peaks of field Damask Rose essential oil; Table 2 is 9 base peak content with field Damask Rose essential oil; 9 kinds of materials that table 3 is and Damask Rose essential oil 9 base peaks in field are corresponding.
demonstration test:
test example 1: the first step: the essential oil 0.025g to 0.030g to be measured extracted with field Damask Rose fresh flower getting the plantation of Bai Shituoge clarke village, Hetian City is placed in test tube, adds normal hexane and be settled to after 10mL shakes up and obtain need testing solution in test tube, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, to calculate and the included angle cosine value obtaining collection of illustrative plates to be measured is 0.9960, and in collection of illustrative plates to be measured, retention time is the content at the corresponding peak of 14.191min is 0.30%, retention time is the content at the corresponding peak of 20.081min is 11.74%, retention time is the content at the corresponding peak of 21.167min is 4.81%, retention time is the content at the corresponding peak of 28.063min is 0.20%, retention time is the content at the corresponding peak of 29.740min is 0.72%, retention time is the content at the corresponding peak of 37.080min is 1.03%, retention time is the content at the corresponding peak of 45.931min is 21.17%, retention time is the content at the corresponding peak of 52.147min is 17.75%, retention time is the content at the corresponding peak of 63.057min is 2.39%, then essential oil to be measured is and field Damask Rose essential oil.Illustrate that testing result conforms to actual by test example 1.
test example 2: the first step: the essential oil 0.025g to 0.030g to be measured extracted with field Damask Rose fresh flower getting the plantation of A Releaike village, Hetian City is placed in test tube, adds normal hexane and be settled to after 10mL shakes up and obtain need testing solution in test tube, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, to calculate and the included angle cosine value obtaining collection of illustrative plates to be measured is 0.9973, and in collection of illustrative plates to be measured, retention time is the content at the corresponding peak of 14.191min is 0.25%, retention time is the content at the corresponding peak of 20.081min is 14.16%, retention time is the content at the corresponding peak of 21.167min is 2.76%, retention time is the content at the corresponding peak of 28.063min is 0.32%, retention time is the content at the corresponding peak of 29.740min is 0.62%, retention time is the content at the corresponding peak of 37.080min is 0.86%, retention time is the content at the corresponding peak of 45.931min is 21.50%, retention time is the content at the corresponding peak of 52.147min is 18.75%, retention time is the content at the corresponding peak of 63.057min is 2.80%, then essential oil to be measured is and field Damask Rose essential oil.Illustrate that testing result conforms to actual by test example 2.
test example 3: the first step: the essential oil 0.025g to 0.030g to be measured that the purple branch rose in Shandong of getting the plantation of Yutian County, Hetian City is extracted is placed in test tube, adds normal hexane and is settled to after 10mL shakes up and obtains need testing solution in test tube, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, calculates and the included angle cosine value obtaining collection of illustrative plates to be measured is 0.6305, in collection of illustrative plates to be measured, retention time is the content at the corresponding peak of 14.191min is 1.005%, retention time is the content at the corresponding peak of 20.081min is 42.27%, retention time is the content at the corresponding peak of 21.167min is 2.26%, retention time is the content at the corresponding peak of 28.063min is 0.08%, retention time is the content at the corresponding peak of 29.740min is 0.11%, retention time is the content at the corresponding peak of 37.080min is 0.22%, retention time is the content at the corresponding peak of 45.931min is 3.40%, retention time is the content at the corresponding peak of 52.147min is 9.42%, retention time is the content at the corresponding peak of 63.057min is 8.57%, then essential oil to be measured is not and field Damask Rose essential oil.Illustrate that testing result conforms to actual by test example 3.
the HP-5MS chromatographic column higher than polyglycol chromatographic column by employing temperature of the property of the present invention is directed to, can detect more high boiling component, obtain more complete detection finger-print, make testing result more accurate, its fingerprint characteristic has been drawn to the foundation of field Damask Rose essential oil GC/MS finger-print and analysis, using spectrogram similarity as evaluation index, from macroscopically controlling and the quality of field Damask Rose essential oil, determine the content range of its property material, fragrant comprising head, body note, bottom note, fixative ingredients and not existing standard pay close attention to body note composition, the more fully overall fragrance of control and field Damask Rose essential oil, composition and the content of high straight chain alkane are paid close attention to, effective control essential oil congealing point, chemically composition controls outward appearance and fragrance more intuitively, formulate the standard of property material quality testing on this basis, thus substantially increase accuracy of detection and detection efficiency, can be used for the quality assessment with field Damask Rose essential oil, for providing a kind of quality standard with the quality control of field Damask Rose essential oil, head sachet draws together linalool, and body note comprises citronellol and geraniol, and bottom note comprises carypohyllene, β-farnesene and sagittol, and fixation comprises nonadecane, heneicosane and pentacosane.
above technical characteristic constitutes embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease non-essential technical characteristic according to actual needs, meet the demand of different situations.
Claims (6)
1. one kind and field Damask Rose essential oil are used for the GC/MS fingerprint atlas detection method of standard, it is characterized in that carrying out as follows: the first step, get 0.025g to 0.030g essential oil to be measured and be placed in test tube, in test tube, add normal hexane be settled to after 10mL shakes up and obtain need testing solution, second step, need testing solution is added in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, collection of illustrative plates to be measured is obtained after mass spectrum, 3rd step, calculates the included angle cosine value of collection of illustrative plates to be measured,
wherein: n=1 ... 133, y
ibe the peak area of the base peak of i-th corresponding retention time, x
ifor the peak area at the peak of i-th corresponding retention time in collection of illustrative plates to be measured, in collection of illustrative plates to be measured corresponding retention time without peak then peak area be 0, if the included angle cosine value of collection of illustrative plates to be measured is less than 0.9246, then essential oil to be measured is not and field Damask Rose essential oil, if included angle cosine value is greater than 0.9246, and to meet retention time in collection of illustrative plates to be measured be the content at the corresponding peak of 14.191min is 0.10% to 0.70% simultaneously, retention time is the content at the corresponding peak of 20.081min is 11.70% to 19.20%, retention time is the content at the corresponding peak of 21.167min is 1.70% to 9.00%, retention time is the content at the corresponding peak of 28.063min is 0.20% to 0.60%, retention time is the content at the corresponding peak of 29.740min is 0.20% to 0.80%, retention time is the content at the corresponding peak of 37.080min is 0.60% to 1.30%, retention time is the content at the corresponding peak of 45.931min is 19.00% to 23.00%, retention time is the content at the corresponding peak of 52.147min is 13.70% to 20.00%, retention time is the content at the corresponding peak of 63.057min is 1.30% to 3.00%, then essential oil to be measured is and field Damask Rose essential oil.
2. according to claim 1 and field Damask Rose essential oil is used for the GC/MS fingerprint atlas detection method of standard, it is characterized in that the peak area of the base peak of corresponding retention time obtains as follows: the first step, gather No. 1 ground respectively, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, 1.5 kilograms to 2 kilograms and field Damask Rose fresh flower that No. 6 ground and the same day of No. 7 planting open, placing respectively in a reservoir with field Damask Rose fresh flower by various places after collection, then the pure water with field Damask Rose fresh flower quality 3 doubly to 4 times is added in a reservoir respectively, refluxing extraction is carried out after being heated to boiling, refluxing extraction 3h to 4h, after refluxing extraction, distillate obtains distillating phase after condenser condenses, the upper strata distillating phase is essential oil layer, the lower floor distillating phase is water layer, be separated the upper strata distillating phase and obtain No. 1 Rosa Damascana respectively, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 Rosa Damascanas, second step, get No. 1 Rosa Damascana of 0.025g to 0.030g, No. 2 Rosa Damascanas, No. 3 Rosa Damascanas, No. 4 Rosa Damascanas, No. 5 Rosa Damascanas, No. 6 Rosa Damascanas and No. 7 rhodamine toners are placed in test tube respectively, in test tube, then add normal hexane be respectively settled to after 10mL shakes up and obtain No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution, 3rd step, by No. 1 solution, No. 2 solution, No. 3 solution, No. 4 solution, No. 5 solution No. 6 solution and No. 7 solution add respectively in Agilent HP-5MS chromatographic column and detect, the GC conditions of Agilent HP-5MS chromatographic column is: carrier gas is He, need testing solution sample size is 1 μ L, injector temperature is 300 DEG C, before post, pressure is 7.6522psi, post flow is 1mL/min, split ratio is 4:1, heating schedule is: stop 2min when being warming up to 50 DEG C, then after 280 DEG C, 5min is stopped with the ramp of 3 DEG C/min, 83.667min altogether, Mass Spectrometry Conditions is: solvent delay 3.00 minutes, sweep limit is 33 to 600, EI ion gun, electron energy is 70eV, electron multiplier voltage is 1424V, ion source temperature is 230 DEG C, level Four bar temperature is 150 DEG C, No. 1 collection of illustrative plates is obtained respectively after mass spectrum, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates, 4th step, obtains the peak area of the base peak of 133 corresponding retention times after being averaged by the peak area value at peak corresponding for i-th retention time in No. 1 collection of illustrative plates, No. 2 collection of illustrative plates, No. 3 collection of illustrative plates, No. 4 collection of illustrative plates, No. 5 collection of illustrative plates, No. 6 collection of illustrative plates and No. 7 collection of illustrative plates respectively.
3. according to claim 2 and field Damask Rose essential oil is used for the GC/MS fingerprint atlas detection method of standard, it is characterized in that in the first step, 8:00 to 9:30 gathers open 1.5 kilograms to 2 kilograms and the field Damask Rose fresh flower on the same day of No. 1 ground, No. 2 ground, No. 3 ground, No. 4 ground, No. 5 ground, No. 6 ground and No. 7 ground plantations in the morning.
4. according to Claims 2 or 3, be used for the GC/MS fingerprint atlas detection method of standard with field Damask Rose essential oil, it is characterized in that No. 1 ground for and Tian Yetai Kyzyl village; No. 2 ground are and La Yika village, field; No. 3 ground are and Bai Shituoge clarke village, field; No. 4 ground are Hetian City; No. 5 ground are allow village with Tian Hadi; No. 6 ground are and A Rele village, field; No. 7 ground are and Ba Shi village too, field.
5. according to claim 1 or 2 or 3, be used for the GC/MS fingerprint atlas detection method of standard with field Damask Rose essential oil, it is characterized in that the column length of Agilent HP-5MS chromatographic column is 30m, column internal diameter is 0.25mm, thickness is 0.25 μm.
6. according to claim 4 and field Damask Rose essential oil is used for the GC/MS fingerprint atlas detection method of standard, it is characterized in that the column length of Agilent HP-5MS chromatographic column is 30m, column internal diameter is 0.25mm, thickness is 0.25 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410622894.8A CN104391054B (en) | 2014-11-08 | 2014-11-08 | The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410622894.8A CN104391054B (en) | 2014-11-08 | 2014-11-08 | The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104391054A CN104391054A (en) | 2015-03-04 |
| CN104391054B true CN104391054B (en) | 2015-11-18 |
Family
ID=52608984
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410622894.8A Active CN104391054B (en) | 2014-11-08 | 2014-11-08 | The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104391054B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105938129A (en) * | 2016-07-08 | 2016-09-14 | 上海应用技术学院 | Pingyin rose essential oil GC chromatographic method |
| CN106248850A (en) * | 2016-08-08 | 2016-12-21 | 云南中烟工业有限责任公司 | A kind of method of Fast Evaluation quality of flavoring essence for tobacco |
| CN107085051B (en) * | 2017-04-19 | 2019-10-25 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of construction method and discrimination method of Huanghua Pear redwood tree species finger-print |
| CN107621513A (en) * | 2017-11-03 | 2018-01-23 | 厦门琥珀日化科技股份有限公司 | A kind of adulterated discrimination method of natural rose essential |
| CN108732289B (en) * | 2018-08-14 | 2020-10-09 | 东莞波顿香料有限公司 | Method for identifying natural citronellol and synthetic citronellol |
| CN111187675B (en) * | 2020-03-10 | 2022-11-25 | 北京市农林科学院 | Method for determining feeding ratio and distillation time of Rosa damascena |
| CN114217002B (en) * | 2021-12-06 | 2023-12-15 | 多特瑞(上海)商贸有限公司 | Method for detecting contents of chamomile azulene and sabinene in chamomile essential oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG39948A1 (en) * | 1985-04-25 | 1986-09-15 | Dimitrov | Gas chromatography method for analysis of essential oil mixture |
| BG65650B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the evaluation of the aroma of tobacco smoke and classification by aroma of types and varieties of tobaccos |
| CN102331476A (en) * | 2011-05-31 | 2012-01-25 | 天津春发食品配料有限公司 | Gas chromatographic fingerprint analysis method for savory flavorings |
| CN102507815A (en) * | 2011-10-27 | 2012-06-20 | 浙江工业大学 | Similarity detection method for chromatographic fingerprint spectrogram |
-
2014
- 2014-11-08 CN CN201410622894.8A patent/CN104391054B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG39948A1 (en) * | 1985-04-25 | 1986-09-15 | Dimitrov | Gas chromatography method for analysis of essential oil mixture |
| BG65650B1 (en) * | 2004-09-01 | 2009-04-30 | Солея ДАНЬО | Method for the evaluation of the aroma of tobacco smoke and classification by aroma of types and varieties of tobaccos |
| CN102331476A (en) * | 2011-05-31 | 2012-01-25 | 天津春发食品配料有限公司 | Gas chromatographic fingerprint analysis method for savory flavorings |
| CN102507815A (en) * | 2011-10-27 | 2012-06-20 | 浙江工业大学 | Similarity detection method for chromatographic fingerprint spectrogram |
Non-Patent Citations (8)
| Title |
|---|
| Essential oils analysis. I. Evaluation of essential oils composition using both GC and MS fingerprints;R. Oprean 等;《Journal of Pharmaceutical and Biomedical Analysis》;19991201;第18卷(第4-5期);第651-657页 * |
| Jens K.S. Møller 等.Electrospray ionization mass spectrometry fi * |
| Jian Hong Zeng 等.Application of the chromatographic fi * |
| ngerprint for quality control of essential oil from GuangXi Curcuma kwangsiensis.《Med Chem Res》.2009,第18卷(第2期),第158-165页. * |
| ngerprinting of essential oils: Spices from the Labiatae family.《Food Chemistry》.2007,第100卷(第3期),第1283-1288页. * |
| 张睿 等.商州产大马士革玫瑰精油研究.《西北植物学报》.2005,第25卷(第7期),第1477-1479页. * |
| 新疆玫瑰精油化学成分的研究;刘玉梅 等;《精细化工》;20020731;第19卷(第7期);第388-389+405 * |
| 王淑敏 等.玫瑰花中挥发油成分的超临界萃取及质谱分析.《质谱学报》.2006,第27卷(第1期),第45-49页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104391054A (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104391054B (en) | The GC/MS fingerprint atlas detection method of standard is used for field Damask Rose essential oil | |
| Cutini et al. | Estimation of leaf area index with the Li-Cor LAI 2000 in deciduous forests | |
| Chang et al. | Radial pattern of sap flow and response to microclimate and soil moisture in Qinghai spruce (Picea crassifolia) in the upper Heihe River Basin of arid northwestern China | |
| Martin et al. | Crown conductance and tree and stand transpiration in a second-growth Abies amabilis forest | |
| Yu et al. | Short-term variability in the dates of the Indian monsoon onset and retreat on the southern and northern slopes of the central Himalayas as determined by precipitation stable isotopes | |
| Song et al. | Spatial–temporal variations of spring drought based on spring-composite index values for the Songnen Plain, Northeast China | |
| Zhongjie et al. | Fraction of incident rainfall within the canopy of a pure stand of Pinus armandii with revised Gash model in the Liupan Mountains of China | |
| Gong et al. | Estimation of evapotranspiration and its components from an apple orchard in northwest China using sap flow and water balance methods | |
| Siddiq et al. | More sensitive response of crown conductance to VPD and larger water consumption in tropical evergreen than in deciduous broadleaf timber trees | |
| Herbst et al. | Comparative measurements of transpiration and canopy conductance in two mixed deciduous woodlands differing in structure and species composition | |
| Zeppel et al. | Long term trends of stand transpiration in a remnant forest during wet and dry years | |
| Hardanto et al. | Oil palm and rubber tree water use patterns: effects of topography and flooding | |
| Zhuang et al. | Dew formation characteristics in the gravel desert ecosystem and its ecological roles on Reaumuria soongorica | |
| Li et al. | Response of Populus euphratica Oliv. sap flow to environmental variables for a desert riparian forest in the Heihe River Basin, Northwest China | |
| Song et al. | Higher canopy transpiration rates induced dieback in poplar (Populus× xiaozhuanica) plantations in a semiarid sandy region of Northeast China | |
| Zhao et al. | Canopy transpiration obtained from leaf transpiration, sap flow and FAO‐56 dual crop coefficient method | |
| Ouyang et al. | Stand‐scale transpiration of a Eucalyptus urophylla× Eucalyptus grandis plantation and its potential hydrological implication | |
| Zhang et al. | Meteorological influences on process-based spatial-temporal pattern of throughfall of a xerophytic shrub in arid lands of northern China | |
| Yu et al. | Responses of riparian forests to flood irrigation in the hyper-arid zone of NW China | |
| Bhatta et al. | A comparison of systematic versus stratified-random sampling design for gradient analyses: a case study in subalpine Himalaya, Nepal | |
| da Silva et al. | Surface energy fluxes and evapotranspiration of a mango orchard grown in a semiarid environment | |
| Tong et al. | Radial and seasonal variation of sap flow and its response to meteorological factors in sandy Pinus sylvestris var. mongolica plantations in the Three North Shelterbelt of China | |
| Giuditta et al. | Measuring changes in forest floor evaporation after prescribed burning in Southern Italy pine plantations | |
| Qian et al. | Adaptive, water-conserving strategies in Hedysarum mongolicum endemic to a desert shrubland ecosystem | |
| Tu et al. | Integrated effects of rainfall regime and canopy structure on interception loss: A comparative modelling analysis for an artificial larch forest |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Huang Rongping Inventor after: Chen Qiupeng Inventor after: Wang Yi Inventor before: Huang Rongping Inventor before: Chen Qiupeng Inventor before: Li Xuefei |
|
| COR | Change of bibliographic data |