CN102539572A - Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence - Google Patents
Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence Download PDFInfo
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- CN102539572A CN102539572A CN2012100016655A CN201210001665A CN102539572A CN 102539572 A CN102539572 A CN 102539572A CN 2012100016655 A CN2012100016655 A CN 2012100016655A CN 201210001665 A CN201210001665 A CN 201210001665A CN 102539572 A CN102539572 A CN 102539572A
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Abstract
The invention provides a method for extracting and detecting rutin and quercetol, which is easy to realize automation, is environment-friendly, and has accurate and reliable measuring result and high sensitivity. The method adopts environment-friendly ionic liquid to replace poisonous organic solvent, and utilizes the high-temperature high-pressure condition in the accelerating solvent extraction technology to quickly extract active constituents such as rutin and quercetol in hawthorn of the traditional Chinese medicine, the extracted extract only needs to be simply processed and then can be directly transferred to a high performance liquid chromatograph separation system, and the processed extract can be detected by a chemiluminescence detector after being completely separated by a C18 column, the appearance condition is excellent, better detection result can be obtained, and the detection limit is low. The method can be used for detecting rutin and quercetol in foods, health products and other solid samples with very low content of rutin and quercetol.
Description
Technical field
The invention provides a kind of method that detects rutin and Quercetin, concrete must saying is a kind of new method of utilizing ionic liquid-accelerated solvent extraction high performance liquid chromatography chemiluminescence detection rutin and Quercetin.
Background technology
Rutin and Quercetin all are the natural flavone compounds, have very strong antioxidation activity, can the delaying human body cell ageing, for health important physical effect and medical value are arranged.All contain rutin and Quercetin in the middle of a variety of Chinese medicines; Common method for distilling mainly contains Suo Shi extraction, ultrasonic assisted extraction or microwave-assisted extraction method etc. at present; But these methods often be not extraction time long be exactly that extraction efficiency is not high; Or troublesome poeration, the extract after the extraction needs loaded down with trivial details further processing.And detection means commonly used mainly is a uv detection method, and this method detectability is higher, is difficult to good mensuration for the component of denier in some medicines.
Summary of the invention
The object of the invention provides a kind of new rutin and the extraction and the assay method of Quercetin.This method at first uses ionic liquid as extraction solvent, packs into after the Chinese medicine sample is suitably handled in the accelerated solvent extraction device, under high-temperature and high-pressure conditions, testing sample is carried out fast automatic extraction then.The extract that obtains is analyzed with chemiluminescence detector after chromatographic system separates through directly getting into after the simple centrifugal treating.
Concrete technical scheme of the present invention is following:
The present invention is a kind of method of utilizing ionic liquid-accelerated solvent extraction to follow the example of to extract rutin and Quercetin in the Chinese medicine and detecting its content; This method is organic extraction agent that the extractant in following the example of as accelerated solvent extraction with ionic liquid replaces environmental pollutions such as methyl alcohol; Under the external condition of HTHP; Rutin and Quercetin in the extraction Chinese medicine rapidly and efficiently; Liquid after the extraction is got supernatant and is directly got into highly effective liquid phase chromatographic system after the high speed centrifugation simple process, utilizes chemiluminescence detector to detect after separating fully.
Ionic liquid of the present invention-accelerated solvent extraction extracts rutin and Quercetin in the Chinese medicine and detects the method for its content, and ionic liquid is used for the accelerated solvent extraction process, the method environmental protection; Ion liquid extraction efficiency is high, and whole process shortens the time greatly than traditional heating and refluxing extraction method, and automaticity is high; The method recovery is good; Reliable and stable, chemiluminescence does not need internal light source as detection means; Its sensitivity will be higher than ultraviolet and fluorescence detector far away, can successfully measure the rutin and the Quercetin of denier in the extract.
Method of the present invention can be applicable to other can be by the assay determination of the effective constituent in the Chinese medicine of ionic liquid-accelerated solvent extraction chemiluminescence detection or other solid and semi-solid sample.
Beneficial effect of the present invention is following:
At first rutin in the Chinese medicine sample and Quercetin are extracted when the present invention measures, separate the back with the C18 post then and detect with chemiluminescence detector with ionic liquid-accelerated solvent extraction system.Utilize the ionic liquid replace organic solvent, make this method environmental protection, and the high temperature and high pressure condition of accelerated solvent extraction has promoted ion liquid extracting power greatly; Simultaneously; The use of chemiluminescence detector makes the sensitivity that detects improve greatly; And because chemiluminescence detection itself has certain selectivity; This just makes its spectrogram disturb than the spectrogram of ultraviolet detection to lack, and is suitable for very much as Chinese medicine the mensuration of trace active principle in the complicated substrate; This law is measured simple, and automaticity is high, and is accurately sensitive; Economic environmental protection can be widely used in food, health products and field of medicaments; This method can high efficiency extraction and the sensitive determination traditional Chinese medicine in rutin and Quercetin, still do not have the report of similar detection method both at home and abroad.
Description of drawings
Fig. 1 is ionic liquid-accelerated solvent extraction high performance liquid chromatography chemiluminescence detection rutin Quercetin standard colour chart (1 μ g/mL);
Be labeled as among Fig. 1: 1-rutin, 2-Quercetin;
Fig. 2 is the chromatogram of Chinese medicine hawthorn;
Be labeled as among Fig. 2: 1-rutin, 2-Quercetin.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further:
Rutin Quercetin concrete steps are following in ionic liquid-accelerated solvent extraction high performance liquid chromatography chemiluminescence detection hawthorn:
1, the preparation of standard solution: accurately take by weighing each 10mg of rutin Quercetin standard specimen, place two 10ml volumetric flasks respectively, after the concussion dissolving, constant volume is to scale;
2, the making of typical curve: the method preparation variable concentrations standard solution that adopts stepwise dilution;
3, ionic liquid-accelerated solvent extraction: pharmacy is bought hawthorn stoning afterwash solarization dry doubling pulverize with comminutor; Cross 40 mesh and collection then; Get a certain amount of hawthorn sample and put into the 34mL abstraction pool of accelerated solvent extraction, add an amount of zeyssatite simultaneously, water soluble ion liquid 1-butyl-3-methylimidazole villaumite is made into certain density solution as spreading agent; As extractant, under the temperature and pressure condition that configures, extract automatically.Liquid after the extraction flows in the receiving flask and collects, with 10000 rev/mins of this extracts after centrifugal 10 minutes the dilution certain multiple directly advance chromatographic system analysis;
4, the mensuration of standard solution and sample: sample size 50 μ L; Get the mixed mark of 1 μ g/mL rutin and Quercetin and the hawthorn actual sample extract after the dilution certain multiple respectively and inject chromatographic analysis system, obtain standard specimen chromatogram (accompanying drawing 1) and sample chromatogram figure (accompanying drawing 2).We can see that the rutin appearance time is approximately 5.8 minutes in the accompanying drawing 1, and the Quercetin appearance time is approximately 9.3 minutes, and the two can well separate, and the peak type is good.Can find out in the accompanying drawing 2 that rutin and Quercetin can record in actual sample, and not receive the interference of complex matrices in the actual sample, can well quantitative test.
5, the selection of luminescence reagent: test the luminescence reagent of different systems, in the hope of reaching best mensuration effect, finally this instance is selected 0.5mM potassium permanganate and 5 * 10
-5The M potassium ferricyanide is as luminescence reagent;
6, the selection of moving phase: test different mobile phase proportioning, confirm as at last: 43% methyl alcohol, 0-8 minute, increased methyl alcohol to 65% in 8-9 minute, keep this ratio to 13 minute then;
7, flow rate pump is 1mL/min, and the peristaltic pump flow velocity is 23 rev/mins, negative high voltage, 800V.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in spirit of the present invention and claim protection domain, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (3)
1. an ionic liquid-accelerated solvent extraction extracts rutin and Quercetin in the Chinese medicine and detects the method for its content; It is characterized in that; This method is organic extraction agent that the extractant in following the example of as accelerated solvent extraction with ionic liquid replaces environmental pollutions such as methyl alcohol; Under the external condition of HTHP, rutin and Quercetin in the extraction Chinese medicine rapidly and efficiently, the liquid after the extraction is after the high speed centrifugation simple process; Get supernatant and directly get into highly effective liquid phase chromatographic system, utilize chemiluminescence detector to detect after separating fully.
2. ionic liquid according to claim 1-accelerated solvent extraction extracts rutin and Quercetin in the Chinese medicine and detects the method for its content, it is characterized in that described ionic liquid is used for the accelerated solvent extraction process; The method environmental protection, ion liquid extraction efficiency is high, and whole process shortens the time greatly than traditional heating and refluxing extraction method; Automaticity is high, and the method recovery is good, and is reliable and stable; Chemiluminescence is as detection means; Do not need internal light source, its sensitivity will be higher than ultraviolet and fluorescence detector far away, can successfully measure the rutin and the Quercetin of denier in the extract.
3. ionic liquid according to claim 1 and 2-accelerated solvent extraction extracts rutin and Quercetin in the Chinese medicine and detects the method for its content; It is characterized in that can be applicable to other can be by the assay determination of the effective constituent in the Chinese medicine of ionic liquid-accelerated solvent extraction chemiluminescence detection or other solid and semi-solid sample.
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| CN2012100016655A CN102539572A (en) | 2012-01-05 | 2012-01-05 | Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102824431A (en) * | 2012-09-06 | 2012-12-19 | 河北科技师范学院 | Method for extracting hawthorn flavone by using pressurized liquid extraction (APLE) technique |
| CN103202851A (en) * | 2013-04-19 | 2013-07-17 | 曹君 | Extraction method of hawthorn active components |
| CN103275145A (en) * | 2013-06-14 | 2013-09-04 | 山东农业大学 | Ultrasonic extraction method for forsythiaside compound by using ionic liquid |
| CN106370494A (en) * | 2016-10-12 | 2017-02-01 | 林圣灼 | Method for extracting and separating coumarin by utilizing [BuPy(Butyl Pyridine)] PF6 |
| CN104359886B (en) * | 2014-11-21 | 2017-04-12 | 南京林业大学 | Application of quercetin to determination of CH3COO＜-＞ as fluorescent probe and method for determining CH3COO＜-＞ |
-
2012
- 2012-01-05 CN CN2012100016655A patent/CN102539572A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 《Talanta》 20111031 Hongwei Wu，et al Determination of rutin and quercetin in Chinese herbal medicine by ionic liquid-based pressurized liquid extraction-liquid chromatography-chemiluminescence detection 1－3 第88卷, * |
| HONGWEI WU，ET AL: "Determination of rutin and quercetin in Chinese herbal medicine by ionic liquid-based pressurized liquid extraction–liquid chromatography–chemiluminescence detection", 《TALANTA》 * |
| 吴宏伟等: "离子色谱分离-化学发光检测槲皮素初探", 《第13届离子色谱学术报告会论文集》 * |
| 程鹏等: "加速溶剂萃取技术提取桑叶中芦丁和槲皮素的工艺研究", 《分析化学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102824431A (en) * | 2012-09-06 | 2012-12-19 | 河北科技师范学院 | Method for extracting hawthorn flavone by using pressurized liquid extraction (APLE) technique |
| CN103202851A (en) * | 2013-04-19 | 2013-07-17 | 曹君 | Extraction method of hawthorn active components |
| CN103275145A (en) * | 2013-06-14 | 2013-09-04 | 山东农业大学 | Ultrasonic extraction method for forsythiaside compound by using ionic liquid |
| CN104359886B (en) * | 2014-11-21 | 2017-04-12 | 南京林业大学 | Application of quercetin to determination of CH3COO＜-＞ as fluorescent probe and method for determining CH3COO＜-＞ |
| CN106370494A (en) * | 2016-10-12 | 2017-02-01 | 林圣灼 | Method for extracting and separating coumarin by utilizing [BuPy(Butyl Pyridine)] PF6 |
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Application publication date: 20120704 |