CN103768828A - Balancing device for solid phase microextraction of fruit fragrance and extraction method - Google Patents
Balancing device for solid phase microextraction of fruit fragrance and extraction method Download PDFInfo
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- CN103768828A CN103768828A CN201410040512.0A CN201410040512A CN103768828A CN 103768828 A CN103768828 A CN 103768828A CN 201410040512 A CN201410040512 A CN 201410040512A CN 103768828 A CN103768828 A CN 103768828A
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Abstract
The invention provides a balancing device for solid phase microextraction of fruit fragrance. The balancing device comprises an ultrasonic cleaner body, wherein an upper cover plate is arranged at the upper end of the ultrasonic cleaner body, an upright post is fixedly arranged in the middle of the top end of the upper cover plate and is horizontally provided with a connecting rod in a sleeved manner, and fixed rings for clamping extraction handles are arranged at two ends of the connecting rod, respectively; extraction holes are formed in the upper cover plate right below the fixed rings, trays for loading head space bottles are arranged below the extraction holes and are fixed at the lower end face of the upper cover plate. The invention further provides a method for carrying out the solid phase microextraction by virtue of the balancing device. The balancing device has the characteristics of high extraction efficiency, strong maneuverability, good test repeatability and the like.
Description
Technical field
The present invention relates to solid phase micro-extraction technique field, be specifically related to a kind of bascule for fruit aroma SPME and extracting process.
Background technology
Fragrance, as an important indicator of fruit quality, not only affects the degree of recognition of market to fruit, also directly affects the quality of its processed goods, is subject in recent years people and more and more pays close attention to.Along with the application of the Modern Analytical Instrument such as gas-chromatography, gas chromatograph-mass spectrometer, fruit aroma also becomes the new focus of fruit quality biological study gradually.
Fruit Aroma is the small molecule organic compound of a class volatilization or half volatile, and the extracting process of science is the prerequisite of Fruit Aroma accurate analysis.The conventional extracting process of Fruit Aroma is headspace solid-phase microextraction at present, it is that centralized procurement sample, extraction, concentrated, sample introduction are integrated, and can with a kind of fruit aroma analytical method of gas chromatography-mass spectrography, it is the aroma substance that head space part that fiber head is placed in to airtight head space bottle is adsorbed fruit tissue volatility or half volatile, in extraction process, often accelerate the balance of aroma substance at extracting head and sample room by methods such as heating, stirrings, after ready to balance, fiber head is taken out and insert gas-chromatography vaporizer, the material adsorbing in thermal desorption coating.Extract in vaporizer after desorb, is imported chromatographic column by mobile phase, completes extraction, separation, concentrated overall process.
Solid-phase micro-extracting device comprises extracting head, handle, wherein extracting head is the vitreous silica fiber head that the 1cm of an outer casing stainless steel tubule is long, scribble different chromatographic stationary phases or adsorbent, extracting head is retractable in stainless steel tube, for extraction, adsorption sample; Handle, for installing or fixed extractor head, can forever use.
Often to promote the balance of aroma substance between sample and extracting head by means of the stirring of magnetic force heating stirrer and heating carrying out fruit aroma SPME.Very loaded down with trivial details in practical operation, before each extraction, all magnetic force rotor to be put into head space bottle, be finished and clean again in order to using next time; And concerning need to adding the fruit sample of extraction heat, water bath device is placed in the magnetic stirring apparatus top of being everlasting, and carrys out Quality control temperature by controlling bath temperature.Extracting head is because of the rocking of head space bottle when extracting on magnetic stirring apparatus, and then the damage such as cause fractureing, and conventionally needs certain device to fix head space bottle, and each extraction all needs to fix, and operates very bothersome.In addition, when rotor rotates in head space bottle, be usually at the base portion of bottle, rotate near the one side of magnetic stirring apparatus heating plate, and usually there is stirring slow or inhomogeneous situation when more in fruit sample, thereby postpone the balance of aroma substance at extracting head and sample room.Different magnetic force heating stirrer and rotor, also often cause the difference of extraction equilibrium time, and whole operating process is subject to the impact of human factor and the repeatability of experiment is reduced.
Therefore a kind of simple, convenient, practical, efficient Fruit Aroma solid phase micro-extraction method tool of invention is of great significance.
Supersonic wave cleaning machine is the high-frequency oscillation signal that utilizes supersonic generator to send, and converts high frequency mechanical oscillation to propagate in medium (water-bath) by transducer.The present invention is intended to utilize ultrasonic wave to replace traditional extracting process, increases operability and the simplicity of extraction, on this basis, invents a kind of simple solid phase micro-extraction method of Fruit Aroma efficiently, has the features such as simple, efficient, stable.
Summary of the invention
In order to address the above problem, the invention provides a kind of bascule for fruit aroma SPME and extracting process, reach the object that extracting operation is simple, efficiency is high and reproducible.
Technical scheme of the present invention is as follows:
A kind of bascule for fruit aroma SPME, comprise supersonic wave cleaning machine body, described supersonic wave cleaning machine body upper end is provided with upper cover plate, in the middle of the top of described upper cover plate, be installed with column, on described column, level is arranged with connecting rod, and the two ends of described connecting rod are respectively equipped with the retainer ring for clamping extraction handle; Be positioned on the upper cover plate under retainer ring and offer extraction aperture, described extraction aperture below is provided with the pallet for loading head space bottle, and described pallet is fixed on the lower surface of upper cover plate.
Further, in the middle of described connecting rod, be provided with lasso, described lasso is enclosed within on described column and is fixed by screwing part.
Further, described retainer ring is provided with and screws part.
Another object of the present invention is to provide a kind of solid phase micro-extraction method, and the method has adopted above-mentioned bascule to extract, and comprises the following steps:
(1) bath temperature that according to extract, supersonic wave cleaning machine is set is to 30-45 ℃, and opening power is heated the temperature value of setting;
(2) the good testing sample of pretreatment is packed in head space bottle, with the pallet of putting into upper cover plate after the sealing of polytetrafluoroethylene (PTFE) lid; Then the extraction handle that extracting head is installed is fixed in retainer ring, and regulates the position of retainer ring that extracting head is inserted in head space bottle;
(3) fiber head of extracting head end is stretched out to extracting head protection tube, start extraction after the ultrasonic time of supersonic wave cleaning machine is set;
(4) after extraction finishes, fiber head is retracted in extracting head protection tube, and its insertion gas chromatograph injection port from bascule takes off is resolved.
In described step (3), the power of supersonic wave cleaning machine is 800w, and its ultrasonic time is 20-30min.
Beneficial effect of the present invention has:
1, extraction efficiency is high: the present invention adopts bascule to extract fruit aroma, has greatly improved extraction efficiency, has saved extraction time.Take the SPME of pear fruit fragrance as example, in 20ml head space bottle, put 10g pulp and carry out extraction and the analysis of aroma substance, while extraction by conventional method, fragrance reaches in extracting head and sample room the time that balance needs 30min left and right; And adopting the inventive method when extraction, its equilibration time is 23-25min.Therefore use of the present invention can be saved the 5-7min time than traditional extraction method at every turn.
2, workable: supersonic wave cleaning machine directly put into by the head space bottle that testing sample is housed by the present invention, utilize hyperacoustic vibration to promote the balance of aroma substance between sample and extracting fiber head, than the method for vibrating at head space bottle with magnetic force rotor in conventional method, easy to use, quick, workable.
3, ease-to-operate is good: the present invention directly controls extraction temperature with the bath temperature in supersonic wave cleaning machine, than conventional method ratio, has lacked special water bath device; Extraction time and temperature all can be undertaken by the microcomputer program of supersonic wave cleaning machine in addition, more easy and simple to handle many than the Artificial Control method in conventional method.
4, favorable repeatability: in the present invention, extraction temperature and time are used microcomputer program control, good stability; Replaced magnetic stirring apparatus and promote the motion of aroma substance in fruit sample with ultrasonic wave, fruit tissue is stressed has evenly reduced the interference of human factor, has increased the repeatability of test.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the side view of upper cover plate in the present invention;
Fig. 3 is the top view of upper cover plate in the present invention;
In figure: 1-supersonic wave cleaning machine body, 2-upper cover plate, 3-connecting rod, 4-column, 5-extracts handle, 6-extracting head, 7-lasso, 8-retainer ring, the little pallet of 9-1, the large pallet of 9-2,10-screws part, 11-extraction aperture.
The specific embodiment
Embodiment mono-:
As shown in Figure 1, 2, 3, a kind of bascule for fruit aroma SPME, comprise supersonic wave cleaning machine body 1, described supersonic wave cleaning machine body 1 upper end is provided with upper cover plate 2, in the middle of the top of described upper cover plate 2, be installed with column 4, on described column 4, level is arranged with connecting rod 3, and the two ends of described connecting rod 3 are respectively equipped with the retainer ring 8 for clamping extraction handle 5; Be positioned on the upper cover plate 2 under retainer ring 8 and offer extraction aperture 11, extraction aperture 11 belows are provided with the little pallet 9-1 and large pallet 9-2 for loading head space bottle, and little pallet 9-1 and large pallet 9-2 are all fixed on the lower surface of upper cover plate.
Further, in the middle of described connecting rod 3, be provided with lasso 7, described lasso 7 is enclosed within on column 4 and by screwing part 10, connecting rod 3 is fixed on column 4.On retainer ring 8, be also provided with and screw part, the handle that extracting head 6 is installed is inserted in retainer ring 8, be then fixed by screwing part.
Embodiment bis-:
Adopt above-mentioned bascule, the method for a kind of pear fruit fragrance SPME, specifically comprises the following steps:
(1) bath temperature that supersonic wave cleaning machine is set is 35 ℃, and opening power is heated 35 ℃;
(2) the Nanguo pear fruit tissue that takes 10g chopping packs in the head space bottle of 20ml, adds the volatilization of 3.6g NaCl(promotion volatile flavor) and internal standard compound 3-nonanone (the 0.04 g ml of 50 μ l
-1) stir evenly, use polytetrafluoroethylene (PTFE) bottle cap sealing, then head space bottle is put into the pallet of upper cover plate, then the extraction handle that extracting head is installed is fixed in retainer ring, and regulate the position of retainer ring that extracting head is inserted in head space bottle;
(3) fiber head of extracting head end is stretched out to extracting head protection tube, the ultrasonic time switch of the supersonic wave cleaning machine that is 800w by power is got to 25min, starts extraction;
(5) after 25min, fiber head is retracted in extracting head protection tube, and by its insertion gas chromatograph injection port from bascule takes off, at 250 ℃, resolve 5min, carry out the analysis of pear fruit fragrance with GC-MS.
Embodiment tri-:
Adopt above-mentioned bascule, a kind of solid phase micro-extraction method of peach juice fragrance, comprises the following steps:
(1) bath temperature that supersonic wave cleaning machine is set is 35 ℃, and opening power is heated 35 ℃;
(2) measure 10ml peach juice and pack in the head space bottle of 20ml, add 3.6g NaCl(to promote the volatilization of volatile flavor) and internal standard compound 3-nonanone (the 0.04 g ml of 50 μ l
-1) stir evenly, use polytetrafluoroethylene (PTFE) bottle cap sealing, then head space bottle is put into the pallet of upper cover plate, then the extraction handle that extracting head is installed is fixed in retainer ring, and regulate the position of retainer ring that extracting head is inserted in head space bottle;
(3) fiber head of extracting head end is stretched out to extracting head protection tube, the ultrasonic time switch of the supersonic wave cleaning machine that is 800w by power is got to 20min, starts extraction;
(5) after 20min, fiber head is retracted in extracting head protection tube, and by its insertion gas chromatograph injection port from bascule takes off, at 250 ℃, resolve 5min, carry out the analysis of pear fruit fragrance with GC-MS.
Embodiment tetra-:
Adopt above-mentioned bascule, a kind of solid phase micro-extraction method of guava juice fragrance, comprises the following steps:
(1) bath temperature that supersonic wave cleaning machine is set is 45 ℃, and opening power is heated 45 ℃;
(2) measure 10 ml fruit juice and pack in the head space bottle of 20ml, add 3.6 g NaCl(to promote the volatilization of volatile flavors) and internal standard compound 3-nonanone (the 0.04 g ml of 25 μ l
-1) stir evenly, use polytetrafluoroethylene (PTFE) bottle cap sealing, then head space bottle is put into the pallet of upper cover plate, then the extraction handle that extracting head is installed is fixed in retainer ring, and regulate the position of retainer ring that extracting head is inserted in head space bottle;
(3) fiber head of extracting head end is stretched out to extracting head protection tube, the ultrasonic time switch of the supersonic wave cleaning machine that is 800w by power is got to 30min, starts extraction;
(5) after 30min, fiber head is retracted in extracting head protection tube, and by its insertion gas chromatograph injection port from bascule takes off, at 250 ℃, resolve 5min, carry out the analysis of pear fruit fragrance with GC-MS.
Above embodiment is not limited only to protection scope of the present invention, all modify based on basic thought of the present invention or change all belong to protection scope of the present invention.
Claims (5)
1. the bascule for fruit aroma SPME, comprise supersonic wave cleaning machine body, it is characterized in that: described supersonic wave cleaning machine body upper end is provided with upper cover plate, in the middle of the top of described upper cover plate, be installed with column, on described column, level is arranged with connecting rod, and the two ends of described connecting rod are respectively equipped with the retainer ring for clamping extraction handle; Be positioned on the upper cover plate under retainer ring and offer extraction aperture, described extraction aperture below is provided with the pallet for loading head space bottle, and described pallet is fixed on the lower surface of upper cover plate.
2. bascule according to claim 1, is characterized in that: in the middle of described connecting rod, be provided with lasso, described lasso is enclosed within on described column and is fixed by screwing part.
3. bascule according to claim 1, is characterized in that: described retainer ring is provided with and screws part.
4. a solid phase micro-extraction method, adopts the bascule as described in claim 1-3 any one, it is characterized in that: comprise the following steps:
(1) bath temperature that according to extract, supersonic wave cleaning machine is set is to 30-45 ℃, and opening power is heated the temperature value of setting;
(2) the good testing sample of pretreatment is packed in head space bottle, with the pallet of putting into upper cover plate after the sealing of polytetrafluoroethylene (PTFE) lid; Then the extraction handle that extracting head is installed is fixed in retainer ring, and regulates the position of retainer ring that extracting head is inserted in head space bottle;
(3) fiber head of extracting head end is stretched out to extracting head protection tube, start extraction after the ultrasonic time of supersonic wave cleaning machine is set;
(4) after extraction finishes, fiber head is retracted in extracting head protection tube, and its insertion gas chromatograph injection port from bascule takes off is resolved.
5. a kind of solid phase micro-extraction method according to claim 4, is characterized in that: in described step (3), the power of supersonic wave cleaning machine is 800w, and its ultrasonic time is 20-30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105806974A (en) * | 2016-03-09 | 2016-07-27 | 西藏大学农牧学院 | Detection method of aroma components of rubus biflorus fruits |
| CN106018630A (en) * | 2016-08-09 | 2016-10-12 | 安徽青松食品有限公司 | Steamed bread flavor substance detection method |
| CN108593822A (en) * | 2018-07-12 | 2018-09-28 | 南京林业大学 | Solid phase microextraction sampling device and its system |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1293376C (en) * | 2004-11-05 | 2007-01-03 | 郑政峯 | Method and device for pretreatment of speeding chemical matter detection |
| CN201637729U (en) * | 2010-04-01 | 2010-11-17 | 复旦大学 | Solid-phase micro-extraction automatic sampling device for determining volatile organic compounds in packing material |
| CN102721766A (en) * | 2011-03-31 | 2012-10-10 | 上海宝钢工业检测公司 | Application of solid phase microextraction in content analysis of naphthalene in Corex furnace gas |
| CN203724814U (en) * | 2014-01-28 | 2014-07-23 | 安徽省农业科学院园艺研究所 | Balancing device for solid phase micro-extraction of fruit aroma |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105806974A (en) * | 2016-03-09 | 2016-07-27 | 西藏大学农牧学院 | Detection method of aroma components of rubus biflorus fruits |
| CN105806974B (en) * | 2016-03-09 | 2017-11-14 | 西藏大学农牧学院 | Rubus biflorus fruit aroma component detection method |
| CN106018630A (en) * | 2016-08-09 | 2016-10-12 | 安徽青松食品有限公司 | Steamed bread flavor substance detection method |
| CN108593822A (en) * | 2018-07-12 | 2018-09-28 | 南京林业大学 | Solid phase microextraction sampling device and its system |
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