CN103768828B - 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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- CN103768828B CN103768828B CN201410040512.0A CN201410040512A CN103768828B CN 103768828 B CN103768828 B CN 103768828B CN 201410040512 A CN201410040512 A CN 201410040512A CN 103768828 B CN103768828 B CN 103768828B
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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, be subject to people in recent years and more and more pay 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 extracting process that current Fruit Aroma is conventional is headspace solid-phase microextraction, it is centralized procurement sample, extraction, concentrated, sample introduction are integrated, and can with a kind of fruit aroma analytical method of gas chromatography-mass spectrography, be fiber head is placed in airtight ml headspace bottle head space part to adsorb the aroma substance of fruit tissue volatility or half volatile, the balance of aroma substance at extracting head and sample room is accelerated usually through methods such as heating, stirrings in extraction process, after ready to balance, fiber head is taken out and insert gas-chromatography vaporizer, the material that thermal desorption coating is adsorbed.Extract after desorb, is imported chromatographic column by mobile phase in vaporizer, completes extracting and developing, 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 is used for installing or fixed extractor head, can forever use.
Carry out fruit aroma SPME often will by means of the stirring of magnetic force heating stirrer and heat promote aroma substance between sample and extracting head balance.Very loaded down with trivial details in practical operation, all magnetic rotor to be put into ml headspace bottle before each extraction, be finished cleaning again and use in order to next time; And concerning the fruit sample needing to add extraction heat, placing water bath device above magnetic stirring apparatus of being everlasting, carrying out Quality control temperature by controlling bath temperature.When extracting on magnetic stirring apparatus, extracting head is rocked because of rocking of ml headspace bottle, and then causes damages such as fractureing, and usually need certain device to fix ml headspace bottle, each extraction all needs to fix, and operates very bothersome.In addition, when rotor rotates in ml headspace bottle, be usually the base portion at bottle, the one side near magnetic stirring apparatus heating plate rotates, and when fruit sample is more, usually occur stirring slow or uneven situation, thus postpone the balance of aroma substance at extracting head and sample room.Different magnetic force heating stirrers 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 utilizing supersonic generator to send, and converts high frequency mechanical oscillation to and 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 solid phase micro-extraction method of simple Fruit Aroma efficiently, has the features such as simple, efficient, stable.
Summary of the invention
In order to solve the 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 with 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, column is installed with in the middle of the top of described upper cover plate, 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 immediately below retainer ring and offer extraction aperture, be provided with the pallet for loading ml headspace bottle below described extraction aperture, described pallet is fixed on the lower surface of upper cover plate.
Further, be provided with lasso in the middle of described connecting rod, described lasso is enclosed within 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, the process employs above-mentioned bascule and extracts, comprise the following steps:
(1) arrange the bath temperature of supersonic wave cleaning machine to 30-45 DEG C according to extract, opening power is heated the temperature value of setting;
(2) testing sample good for pretreatment is loaded in ml headspace bottle, with the pallet putting into upper cover plate after the sealing of polytetrafluoroethylene (PTFE) lid; Then the extraction handle being provided with extracting head is fixed in retainer ring, and regulates the position of retainer ring to make extracting head insert in ml headspace bottle;
(3) fiber head of extracting head end is stretched out extracting head protection tube, after the ultrasonic time of supersonic wave cleaning machine is set, start extraction;
(4) after extraction terminates, in extracting head that fiber head is retracted protection tube, and it is taken off rear insertion gas chromatograph injection port from bascule resolve.
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, drastically increases extraction efficiency, has saved extraction time.For the SPME of pear fruit fragrance, in 20ml ml headspace bottle, put extraction and analysis that 10g pulp carries out aroma substance, when extracting by conventional method, fragrance reaches the time balancing and need about 30min in extracting head and sample room; And when adopting the inventive method to extract, its equilibration time is 23-25min.Therefore use of the present invention is more each than conventional extraction process saves the 5-7min time.
2, workable: the ml headspace bottle that testing sample is housed directly is put into supersonic wave cleaning machine by the present invention, utilize hyperacoustic vibration to promote the balance of aroma substance between sample and extracting fiber head, than the method for carrying out in ml headspace bottle by magnetic rotor in conventional method vibrating, 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 are all 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 control with microcomputer program, good stability; Instead of with ultrasonic wave the motion that magnetic stirring apparatus promotes aroma substance in fruit sample, fruit tissue uniform force, decrease the interference of human factor, add 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, and 10-screws part, 11-extraction aperture.
Detailed description of the invention
Embodiment one:
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, column 4 is installed with in the middle of the top of described upper cover plate 2, 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; Being positioned on the upper cover plate 2 immediately below retainer ring 8 and offering extraction aperture 11, being provided with the little pallet 9-1 for loading ml headspace bottle and large pallet 9-2 below extraction aperture 11, little pallet 9-1 and large pallet 9-2 is all fixed on the lower surface of upper cover plate.
Further, be provided with lasso 7 in the middle of described connecting rod 3, described lasso 7 is enclosed within column 4 and is fixed on column 4 by connecting rod 3 by screwing part 10.Retainer ring 8 being also provided with and screwing part, the handle being provided with extracting head 6 is inserted in retainer ring 8, being then fixed by screwing part.
Embodiment two:
Adopt above-mentioned bascule, the method for a kind of pear fruit fragrance SPME, specifically comprises the following steps:
(1) bath temperature arranging supersonic wave cleaning machine is 35 DEG C, and opening power is heated 35 DEG C;
(2) the Nanguo pear fruit tissue taking 10g chopping loads in the ml headspace 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 ml headspace bottle is put into the pallet of upper cover plate, then the extraction handle being provided with extracting head is fixed in retainer ring, and regulate the position of retainer ring to make extracting head insert in ml headspace bottle;
(3) fiber head of extracting head end being stretched out extracting head protection tube, is that 25min got to by the ultrasonic time switch of the supersonic wave cleaning machine of 800w by power, starts extraction;
(5) after 25min, in extracting head of being retracted by fiber head protection tube, and it is taken off rear insertion gas chromatograph injection port from bascule, at 250 DEG C, carry out parsing 5min, carry out the analysis of pear fruit fragrance with GC-MS.
Embodiment three:
Adopt above-mentioned bascule, a kind of solid phase micro-extraction method of peach juice fragrance, comprises the following steps:
(1) bath temperature arranging supersonic wave cleaning machine is 35 DEG C, and opening power is heated 35 DEG C;
(2) measure 10ml peach juice to load in the ml headspace bottle of 20ml, add 3.6g NaCl(and 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 ml headspace bottle is put into the pallet of upper cover plate, then the extraction handle being provided with extracting head is fixed in retainer ring, and regulate the position of retainer ring to make extracting head insert in ml headspace bottle;
(3) fiber head of extracting head end being stretched out extracting head protection tube, is that 20min got to by the ultrasonic time switch of the supersonic wave cleaning machine of 800w by power, starts extraction;
(5) after 20min, in extracting head of being retracted by fiber head protection tube, and it is taken off rear insertion gas chromatograph injection port from bascule, at 250 DEG C, carry out parsing 5min, carry out the analysis of pear fruit fragrance with GC-MS.
Embodiment four:
Adopt above-mentioned bascule, a kind of solid phase micro-extraction method of guava juice fragrance, comprises the following steps:
(1) bath temperature arranging supersonic wave cleaning machine is 45 DEG C, and opening power is heated 45 DEG C;
(2) measure 10 ml fruit juice to load in the ml headspace bottle of 20ml, add 3.6 g NaCl(and 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 ml headspace bottle is put into the pallet of upper cover plate, then the extraction handle being provided with extracting head is fixed in retainer ring, and regulate the position of retainer ring to make extracting head insert in ml headspace bottle;
(3) fiber head of extracting head end being stretched out extracting head protection tube, is that 30min got to by the ultrasonic time switch of the supersonic wave cleaning machine of 800w by power, starts extraction;
(5) after 30min, in extracting head of being retracted by fiber head protection tube, and it is taken off rear insertion gas chromatograph injection port from bascule, at 250 DEG C, carry out parsing 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, column is installed with in the middle of the top of described upper cover plate, 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 immediately below retainer ring and offer extraction aperture, be provided with the pallet for loading ml headspace bottle below described extraction aperture, described pallet is fixed on the lower surface of upper cover plate.
2. bascule according to claim 1, is characterized in that: be provided with lasso in the middle of described connecting rod, described lasso is enclosed within 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 any one of claim 1-3, it is characterized in that: comprise the following steps:
(1) arrange the bath temperature of supersonic wave cleaning machine to 30-45 DEG C according to extract, opening power is heated the temperature value of setting;
(2) testing sample good for pretreatment is loaded in ml headspace bottle, with the pallet putting into upper cover plate after the sealing of polytetrafluoroethylene (PTFE) lid; Then the extraction handle being provided with extracting head is fixed in retainer ring, and regulates the position of retainer ring to make extracting head insert in ml headspace bottle;
(3) fiber head of extracting head end is stretched out extracting head protection tube, after the ultrasonic time of supersonic wave cleaning machine is set, start extraction;
(4) after extraction terminates, in extracting head that fiber head is retracted protection tube, and it is taken off rear insertion gas chromatograph injection port from bascule resolve.
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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| 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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| CN1616945A (en) * | 2004-11-05 | 2005-05-18 | 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616945A (en) * | 2004-11-05 | 2005-05-18 | 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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