CN105866081A - Detection method for L-borneol - Google Patents
Detection method for L-borneol Download PDFInfo
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- CN105866081A CN105866081A CN201610209318.XA CN201610209318A CN105866081A CN 105866081 A CN105866081 A CN 105866081A CN 201610209318 A CN201610209318 A CN 201610209318A CN 105866081 A CN105866081 A CN 105866081A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention discloses a detection method for L-borneol. According to the detection method, a supermolecule complex prepared from cucurbit [8] urils and proflavine is taken as a probe S and the probe S is used for performing qualitative and quantitative detection on L-borneol. The detection method specifically comprises the following three steps: preparing the probe S and the L-borneol standard solution, drawing a standard curve and determining a sample. The detection method for L-borneol has the characteristics of no requirement for expensive instrument, low analysis cost, simplicity, sensitivity and high speed.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to the detection method of a kind of L-Borneol.
Background technology
L-Borneol is the fresh leaf extract of feverfew Blumea balsamifera, is commonly used for Chinese patent drug, high-grade spices and food
In blending additive, in view of L-Borneol have antibacterial, anti-inflammatory, invigorate blood circulation, dispel the wind, the effect such as detumescence, therefore, measure L-Borneol
Content to study its Related product effect significant.
Due to its design feature, L-Borneol does not have ultraviolet and fluorescence spectrum.At present, the L-Borneol analysis reported
Method mainly uses capillary gas chromatography and high performance liquid chromatography, and these detection methods exist detecting instrument costliness, sample
Product complex pretreatment, analysis cost are high and organic solvent uses too much problem.Therefore, design is a kind of simple, sensitive, quick
L-Borneol detection method is the most necessary.
Fluorescent molecular probe, owing to having that high sensitivity, testing cost be cheap, sample treatment and simple to operate, mensuration side
Method is quick, enjoy favor without expensive instrument and equipment, the easily advantage such as realization visualization and detection in real time.At present, there is not yet profit
Relevant report with fluorescence probe detection L-Borneol.
Summary of the invention
It is an object of the invention to provide one relatively low and simple, sensitive, quickly left without expensive instrument, analysis cost
The detection method of rotation borneol.
The detection method of a kind of L-Borneol of the present invention, the method utilization prepares with eight yuan of melon rings and proflavin
Super molecular complex, as probe S, carries out qualitative and quantitative detection with this probe S to L-Borneol, specifically includes following steps:
(1) fluorescence probe S and the preparation of L-Borneol standard liquid:
Accurately weigh eight yuan of melon rings of 15.1mg to mix with 4.9mg proflavin, be configured to 100 ml, eight yuan of melon rings with redistilled water
With proflavin molar concentration rate be 1:2, molar concentration be 1.0 × 10-4The fluorescence probe S solution of mol/L;
Accurately weigh 7.7mg L-Borneol, with the second distillation aqueous solution be configured to 500ml, molar concentration is 1.0 × 10-4
The L-Borneol standard liquid of mol/L;
(2) drafting of calibration curve:
Taking 7,10 ml volumetric flask, every bottle adds 1.0 × 10-4After mol/L fluorescence probe S solution 500ul, the most accurately add
0、50.0、100.0、150.0、200.0、250.0、300.0ul 1.0×10-4Mol/L L-Borneol standard liquid, steams with secondary
Distilled water is settled to scale, shakes up, and after room temperature places 10-20min, fixing excitation wavelength 443nm carries out fluorescence emission spectrum mensuration,
With L-Borneol concentration as abscissa, under corresponding 511nm, fluorescence emission spectral intensity is that ordinate draws calibration curve;
(3) mensuration of sample:
I, sample pre-treatments: take the conventional products 2ml containing L-Borneol in composition, adds the mixing of 20ml absolute ethyl alcohol, adds
3-5 g anhydrous sodium sulfate is dried, collected by suction filtrate of reducing pressure, by gained filtrate in 45 DEG C of rotary evaporation recycling design of water-bath,
Extract;Extract is shaken 5-15min with 10ml redistilled water whirlpool, obtains sample solution;
II, sample detection:
A) calibration curve method: take 3,10ml volumetric flask, is separately added into 50ul and shakes 5-15min with 10ml redistilled water whirlpool
After the sample solution that obtains and 500ul 1.0 × 10-4Mol/L fluorescence probe S solution, is settled to scale with redistilled water, shakes
Even, after room temperature places 10-20min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, root
On calibration curve, find the concentration of L-Borneol in sample solution, experiment parallel determination 3 times according to fluorescence intensity, average;
B) standard addition method: take 5,10 ml volumetric flask, is separately added into 50ul and shakes 5-15min with 10ml redistilled water whirlpool
After obtain sample solution, 500ul 1.0 × 10-4After mol/L fluorescence probe S solution, be sequentially added into 0,25.0,50.0,75.0,
100.0ul 1.0×10-4Mol/L L-Borneol standard liquid, is settled to scale with redistilled water, shakes up, and room temperature is placed
After 10-20min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, according to fluorescence intensity
Draw calibration curve, extend the intersection point of calibration curve and abscissa, calculate the content of L-Borneol in sample solution, test parallel
Measure 3 times, average.
The detection method of above-mentioned a kind of L-Borneol, wherein: described calibration curve linear equation is: If=0.50c+
42.8, L-Borneol detection is limited to 5.12 × 10-8Mol/L, the range of linearity is 0.0-3.0 × 10-6mol/L。
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions: the present invention be based on
Eight yuan of melon rings can make the fluorescence generation quencher of proflavin thus form super molecular complex fluorescence probe S, when in fluorescence probe S
After adding L-Borneol, L-Borneol and probe S form new ternary complex, make the fluorescence of quencher be restored, utilize this
The fluorescent switch effect of kind super molecular compound, thus the detection method of a kind of L-Borneol set up.
In aqueous, the fluorescence probe S of individualism, fixing excitation wavelength 443nm, slit 5nm, glimmering during voltage 550v
It is weak that light launches fluorescence intensity level at wavelength 511nm, L-Borneol unstressed configuration spectral quality, after adding L-Borneol in probe S,
At solution fluorescence emission spectrum correspondence 511nm, fluorescent emission intensity is remarkably reinforced, and observes yellow green under 365nm uviol lamp
Hyperfluorescence, result shows that probe S has recognition detection performance to L-Borneol.By under the same conditions, left-handed in probe S+
The borneol aqueous solution adds interfering material that may be present (camphor, ethanol, polyethylene glycol) and contrasts the reality of fluorescent emission intensity afterwards
Testing and show, this fluorophor cording has certain anti-interference.
The detection method of L-Borneol provided by the present invention relatively conventional capillary gas chromatography, high performance liquid chromatography
Detection L-Borneol is the quickest, simple, sensitive, and is capable of the rapid field detection of gross sample.
Accompanying drawing explanation
Fig. 1 be fluorescence probe S solution fluorescence spectroscopic methodology detection L-Borneol canonical plotting (excitation wavelength is 443nm,
Slit 5nm, voltage 550v);
Fig. 2 is the interfering material that may be present interference experiment figure to system.
Detailed description of the invention
Experimental result is coordinated to further illustrate beneficial effects of the present invention below by embodiment.
The detection method of a kind of L-Borneol, comprises the following steps:
(1) fluorescence probe S and the preparation of L-Borneol standard liquid:
Accurately weigh eight yuan of melon rings of 15.1mg to mix with 4.9mg proflavin, be configured to 100 ml, eight yuan of melon rings with redistilled water
With proflavin molar concentration rate be 1:2, molar concentration be 1.0 × 10-4The fluorescence probe S solution of mol/L;
Accurately weigh 7.7mg L-Borneol, with the second distillation aqueous solution be configured to 500ml, molar concentration is 1.0 × 10-4
The L-Borneol standard liquid of mol/L;
(2) drafting of calibration curve:
Taking 7,10 ml volumetric flask, every bottle adds 1.0 × 10-4After mol/L fluorescence probe S solution 500ul, the most accurately add
Enter 0,50.0,100.0,150.0,200.0,250.0,300.0ul 1.0 × 10-4Mol/L L-Borneol standard liquid, uses secondary
Distilled water is settled to scale, shakes up, and after room temperature places 10min, fixing excitation wavelength 443nm carries out fluorescence emission spectrum mensuration,
Often group experiment parallel determination three times, with L-Borneol concentration as abscissa, fluorescence emission spectrum under 511nm in corresponding three experiments
Average strength is that ordinate draws calibration curve.
Test result indicate that, the concentration range of linearity of L-Borneol response is 0.0-3.0 × 10-6Mol/L, detection is limited to
5.12×10-8Mol/L, the L-Borneol of variable concentrations can make the fluorescence intensity of system that enhancing in various degree, the method occur
Can be used for the quantitative detection of L-Borneol.See Fig. 1.
Note: after being settled to scale with redistilled water, shake up in above-mentioned Specification Curve of Increasing, the time tune that room temperature is placed
Whole for 15min or 20min, all can get identical experimental result.
(3) mensuration of sample:
I, sample pre-treatments: take the air freshener 2ml containing L-Borneol in composition, adds the mixing of 20ml absolute ethyl alcohol, then adds
Enter 3g anhydrous sodium sulfate to be dried, collected by suction filtrate of reducing pressure, by gained filtrate in 45 DEG C of rotary evaporation recycling design of water-bath, must carry
Take thing;Manner described above parallel processing is final obtains two parts of extracts, and a copy of it shakes 5min, another part with 10ml acetonitrile whirlpool
Shake 5min with 10ml redistilled water whirlpool, obtain sample solution;
II, sample detection:
A) high performance liquid chromatography: by the sample solution sample presentation to obtain after 10ml acetonitrile whirlpool concussion 5min, with efficient liquid phase
The content of chromatography determination wherein L-Borneol;
B) calibration curve method: take 3,10ml volumetric flask, is separately added into 50ul to obtain after 10ml redistilled water whirlpool concussion 5min
The sample solution arrived and 500ul 1.0 × 10-4Mol/L fluorescence probe S solution, is settled to scale with redistilled water, shakes up, room
After temperature places 10min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, strong according to fluorescence
Degree finds the concentration of L-Borneol in sample solution, experiment parallel determination 3 times on calibration curve, averages;
C) standard addition method: take 5,10 ml volumetric flask, be separately added into 50ul with 10ml redistilled water whirlpool concussion 5min after
The sample solution that obtains, 500ul 1.0 × 10-4After mol/L fluorescence probe S solution, be sequentially added into 0,25.0,50.0,75.0,
100.0ul 1.0×10-4Mol/L L-Borneol standard liquid, is settled to scale with redistilled water, shakes up, and room temperature is placed
After 10min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, draw according to fluorescence intensity
Calibration curve, extends the intersection point of calibration curve and abscissa, calculates the content of L-Borneol in sample solution, tests parallel determination
3 times, average.
Testing result see table.
Use calibration curve method and standard addition method that L-Borneol assay result in sample is shown, the present invention and biography
System high performance liquid chromatography testing result is consistent, and method reappearance is preferable.
Note: by the Mass adjust-ment of anhydrous sodium sulfate in above-mentioned sample detection be 4g or 5g, whirlpool concussion time be adjusted to
The time that 10min or 15min, room temperature are placed is adjusted to 15min or 20min, all can get identical experimental result.
(4) interfering material interference experiment to system:
Interfering material that may be present (camphor, ethanol, polyethylene glycol) is weighed appropriate redistilled water and is configured to the denseest
The standard liquid of degree.
A) adding concentration in 10.0 ml volumetric flasks is 1.0 × 10-4Mol/L fluorescence probe S solution 0.5ml, 1.0 ×
10-4Mol/L L-Borneol standard liquid 0.5ml, redistilled water is settled to scale, shakes up, room temperature placement 10 minutes, now
Fluorescence probe S, L-Borneol molar concentration rate is 1:1;
B) adding concentration in 10.0 ml volumetric flasks is 1.0 × 10-4Mol/L fluorescence probe S solution 0.5 ml, 1.0 × 10-4
Mol/L L-Borneol standard liquid 0.5ml, and 1.0 × 10-4Mol/L camphor standard liquid 0.2ml, redistilled water is fixed
Holding to scale, shake up, room temperature is placed 10 minutes;Adding concentration in 10.0 ml volumetric flasks is 1.0 × 10-4Mol/L fluorescence is visited
Pin S solution 0.5 ml, 1.0 × 10-4Mol/L L-Borneol standard liquid 0.5ml, and 1.0 × 10-2Mol/L ethanol mark
Quasi-solution 0.5ml, redistilled water is settled to scale, shakes up, and room temperature is placed 10 minutes;10.0 ml volumetric flasks add dense
Degree is 1.0 × 10-4The mol/L probe S aqueous solution 0.5 ml, 1.0 × 10-4Mol/L L-Borneol standard liquid 0.5ml, with
And 5.0 × 10-3Mol/L polyethylene glycol standard liquid 1ml, redistilled water is settled to scale, shakes up, and room temperature is placed 10 minutes;
Fixing identical excitation wavelength 443nm, slit 5nm, voltage 550v, measure two groups of solution fluorescence emission spectrum under 511nm strong
Degree, often group experiment parallel determination 3 times, average.
Test result indicate that, when camphor concentration is less than 2 μMs, and ethanol, polyethyleneglycol content are 100 times of L-Borneol content
Time, the detection to L-Borneol does not interferes.See Fig. 2.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, Ren Hewei
Depart from technical solution of the present invention content, any simple modification of above example being made according to the technical spirit of the present invention, etc.
With change and modification, all still fall within the range of technical solution of the present invention.
Claims (2)
1. the detection method of a L-Borneol, it is characterised in that: utilize the oversubscription prepared with eight yuan of melon rings with proflavin
Sub-complex, as probe S, carries out qualitative and quantitative detection with this probe S to L-Borneol, specifically includes following steps:
(1) fluorescence probe S and the preparation of L-Borneol standard liquid:
Accurately weigh eight yuan of melon rings of 15.1mg to mix with 4.9mg proflavin, be configured to 100 ml, eight yuan of melon rings with redistilled water
With proflavin molar concentration rate be 1:2, molar concentration be 1.0 × 10-4The fluorescence probe S solution of mol/L;
Accurately weigh 7.7mg L-Borneol, with the second distillation aqueous solution be configured to 500ml, molar concentration is 1.0 × 10-4 mol/
The L-Borneol standard liquid of L;
(2) drafting of calibration curve:
Taking 7,10 ml volumetric flask, every bottle adds 1.0 × 10-4After mol/L fluorescence probe S solution 500ul, the most accurately add
0、50.0、100.0、150.0、200.0、250.0、300.0ul 1.0×10-4Mol/L L-Borneol standard liquid, steams with secondary
Distilled water is settled to scale, shakes up, and after room temperature places 10-20min, fixing excitation wavelength 443nm carries out fluorescence emission spectrum mensuration,
With L-Borneol concentration as abscissa, under corresponding 511nm, fluorescence emission spectral intensity is that ordinate draws calibration curve;
(3) mensuration of sample:
I, sample pre-treatments: take the conventional products 2ml containing L-Borneol in composition, adds the mixing of 20ml absolute ethyl alcohol, adds
3-5 g anhydrous sodium sulfate is dried, collected by suction filtrate of reducing pressure, by gained filtrate in 45 DEG C of rotary evaporation recycling design of water-bath,
Extract;Extract is shaken 5-15min with 10ml redistilled water whirlpool, obtains sample solution;
II, sample detection:
A) calibration curve method: take 3,10ml volumetric flask, is separately added into 50ul and shakes 5-15min with 10ml redistilled water whirlpool
After the sample solution that obtains and 500ul 1.0 × 10-4Mol/L fluorescence probe S solution, is settled to scale with redistilled water, shakes
Even, after room temperature places 10-20min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, root
On calibration curve, find the concentration of L-Borneol in sample solution, experiment parallel determination 3 times according to fluorescence intensity, average;
B) standard addition method: take 5,10 ml volumetric flask, is separately added into 50ul and shakes 5-15min with 10ml redistilled water whirlpool
After obtain sample solution, 500ul 1.0 × 10-4After mol/L fluorescence probe S solution, be sequentially added into 0,25.0,50.0,75.0,
100.0ul 1.0×10-4Mol/L L-Borneol standard liquid, is settled to scale with redistilled water, shakes up, and room temperature is placed
After 10-20min, fixing excitation wavelength 443nm, launch wavelength 511nm, measure fluorescence emission spectral intensity, according to fluorescence intensity
Draw calibration curve, extend the intersection point of calibration curve and abscissa, calculate the content of L-Borneol in sample solution, test parallel
Measure 3 times, average.
The detection method of a kind of L-Borneol the most as claimed in claim 1, it is characterised in that: described calibration curve linear equation
For: If=0.50c+42.8, L-Borneol detection is limited to 5.12 × 10-8Mol/L, the range of linearity is 0.0-3.0 × 10-6mol/L。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106596490A (en) * | 2016-12-20 | 2017-04-26 | 中国农业大学 | Supermolecular sensor array and method for synchronously detecting paraquat and diquat |
CN110559676A (en) * | 2019-08-29 | 2019-12-13 | 南通东概念新材料有限公司 | System and method for monitoring volume of rotary evaporation liquid in real time by using laser calibration method |
-
2016
- 2016-04-06 CN CN201610209318.XA patent/CN105866081B/en not_active Expired - Fee Related
Non-Patent Citations (4)
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MIGUEL A. ROMERO ET AL.: "Terpenes Show Nanomolar Affinity and Selective Binding with Cucurbit[8]uril", 《ISRAEL JOURNAL OF CHEMISTRY》 * |
席芸芸: "瓜环_染料荧光探针的构筑及检测性能研究", 《中国优秀硕士学位论文全文数据库·工程科技Ⅰ辑》 * |
张静,唐青 等: "超分子荧光探针对水中敌草快的识别与检测", 《广西大学学报(自然科学版)》 * |
王秀林,张丽君等: "盐酸小檗碱含量测定的荧光新方法研究", 《分析测试学报》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106596490A (en) * | 2016-12-20 | 2017-04-26 | 中国农业大学 | Supermolecular sensor array and method for synchronously detecting paraquat and diquat |
CN106596490B (en) * | 2016-12-20 | 2018-12-18 | 中国农业大学 | The supermolecule sensor array and method of synchronous detection paraquat and diquat dibromide |
CN110559676A (en) * | 2019-08-29 | 2019-12-13 | 南通东概念新材料有限公司 | System and method for monitoring volume of rotary evaporation liquid in real time by using laser calibration method |
CN110559676B (en) * | 2019-08-29 | 2024-04-09 | 南通东概念新材料有限公司 | System and method for monitoring volume of rotary evaporation liquid in real time by laser calibration method |
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