CN103884702B - The assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride - Google Patents
The assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride Download PDFInfo
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- CN103884702B CN103884702B CN201410144714.XA CN201410144714A CN103884702B CN 103884702 B CN103884702 B CN 103884702B CN 201410144714 A CN201410144714 A CN 201410144714A CN 103884702 B CN103884702 B CN 103884702B
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- volatile oil
- supernatant liquor
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Abstract
The present invention relates to Baizhu volatile oil inclusion compound field of quality control, the specifically assay method of volatile oil content in a kind of Baizhu volatile oil/Benexate Hydrochloride, the step of this assay method is: I. in inclusion compound, volatile oil ethanol takes off the preparation of bag solution: precision takes Baizhu volatile oil/Benexate Hydrochloride, add absolute ethyl alcohol, ultrasonic 10min, refrigeration 24h; Subsequently with 2500r/min rotating speed, centrifugal 10min, gets supernatant liquor; The mass volume ratio of inclusion compound and absolute ethyl alcohol is 3:1; II. fluorescence analysis is carried out to supernatant liquor.The assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride of the present invention, simple to operation, analyze fast, only need minute quantity sample, mensuration sensitivity is high, reproducible, carry out volatile oil fluorescence analysis method in the forward and backward Baizhu volatile oil/Benexate Hydrochloride of oxygenolysis, thus obtain the index such as inclusion rate, oil content of inclusion compound.
Description
Technical field
The present invention relates to Baizhu volatile oil inclusion compound field of quality control, specifically the assay method of volatile oil content in a kind of Baizhu volatile oil/Benexate Hydrochloride.
Background technology
Baizhu volatile oil traditionally/cyclodextrin inclusion compound assay uses steam distillation.Although the method is widely applied, its heat time is long, large to instability composition influence in volatile oil, and the sample size of needs is also large, tests length consuming time, and operation relative complex, experimental error is large.
Therefore, need badly a kind of simple to operation, analyze and fast, only need minute quantity sample, measure highly sensitive and reproducible assay method Quality Control is realized to Baizhu volatile oil inclusion compound.
Summary of the invention
The present invention is directed to Baizhu volatile oil and there is the volatile general character of volatile oil material, provide the assay method of volatile oil content in this kind of Baizhu volatile oil/Benexate Hydrochloride.
The present invention is achieved by the following technical solutions: the assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride, described Baizhu volatile oil is the volatile oil before oxygenolysis or the volatile oil after oxygenolysis, volatile oil after described oxygenolysis is: the volatile oil before oxygenolysis is after oxygenolysis, and wherein the resolution ratio of atractylone reaches the Baizhu volatile oil of 100%;
The step of this assay method is:
I. in inclusion compound, volatile oil ethanol takes off the preparation of bag solution: precision takes Baizhu volatile oil/Benexate Hydrochloride, adds absolute ethyl alcohol, ultrasonic 10min, refrigeration 24h; Subsequently with 2500r/min rotating speed, centrifugal 10min, gets supernatant liquor; The mass volume ratio of inclusion compound and absolute ethyl alcohol is 3:1;
II. fluorescence analysis is carried out to supernatant liquor:
If a. Baizhu volatile oil is the volatile oil before oxygenolysis, fluorescence condition is: take 429nm as emission wavelength, and with any wavelength within the scope of 340 ~ 409nm for excitation wavelength, slit width is 5nm, and fluorescence analysis obtains its fluorescence intensity F;
If 1. excitation wavelength is 367nm, its fluorescence intensity is F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (1)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，=44.23C
，+9.30（1）
In formula (1): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If 2. excitation wavelength is other wavelength, its fluorescence intensity is F
,, reduce multiple B=F
,/ F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (2)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，，=（44.23C
，，+9.30）/B（2）
In formula (2): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If b. Baizhu volatile oil is the volatile oil after oxygenolysis, fluorescence condition is: take 485nm as emission wavelength, and with any wavelength within the scope of 315 ~ 465nm for excitation wavelength, slit width is 5nm, and fluorescence analysis obtains its fluorescence intensity F;
If 1. excitation wavelength is 396nm, its fluorescence intensity is F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (3)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，=38.68C
，+7.01（3）
In formula (3): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If 2. excitation wavelength is other wavelength, its fluorescence intensity is F
,, reduce multiple B=F
,/ F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (4)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，，=（38.68C
，，+7.01）/B（4）
In formula (4): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor.
Baizhu volatile oil/Benexate Hydrochloride described in the present invention obtains by inclusion compound preparation methods such as polishing well known in the art or ultrasonic methods.
Volatile oil before described oxygenolysis is the volatile oil extracted in Rhizoma Atractylodis Macrocephalae.
The mass volume ratio of step I inclusion compound and absolute ethyl alcohol is 3:1(W/V), this ratio is comparatively in other ratios, high according to the volatile oil content data accuracy that its fluorescence intensity calculates; If other ratios, then in supernatant liquor, the content value of volatile oil may not within the range of linearity of typical curve, if still according to the content of volatile oil in each formulae discovery inclusion compound of the present invention, can impact the accuracy of result of calculation.
Step I of the present invention, according to β-CD(beta-schardinger dextrin-) be slightly soluble in absolute ethyl alcohol, Baizhu volatile oil is soluble in absolute ethyl alcohol, is dissociated out by the Baizhu volatile oil in Baizhu volatile oil/Benexate Hydrochloride by the parameter in step I.
Step II of the present invention has the feature of strong fluorescent emission according to volatile oil ethanolic solution, according to the volatile oil before oxygenolysis and the volatile oil heterogeneity feature after oxygenolysis, different fluorescence analysis conditions is set, and according to the formula that inventor concentrates on studies, try to achieve volatile oil content in volatile oil ethanolic solution (supernatant liquor), and then obtain volatile oil content in inclusion compound.
For the volatile oil before oxygenolysis, inventor thinks that any wavelength within the scope of 340 ~ 409nm is that excitation wavelength all can adopt.Because emission wavelength is 429nm, if excitation wavelength is greater than 409nm, excitation wavelength and emission wavelength values are apart from too little, and both may disturb mutually, affect the accuracy of fluorescence intensity level; If excitation wavelength is less than 340nm, then excitation wavelength is not within the scope of whole excitation peak, and fluorescence intensity level is too little, do not reach the requirement of assay.
For the volatile oil after oxygenolysis, inventor thinks that any wavelength within the scope of 315 ~ 465nm is that excitation wavelength all can adopt, and the value reason of the excitation wavelength within the scope of this is the same.
The assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride of the present invention, simple to operation, analyze fast, only need minute quantity sample, mensuration sensitivity is high, reproducible, absolute ethyl alcohol is slightly soluble according to β-CD, Baizhu volatile oil is soluble in absolute ethyl alcohol, and volatile oil ethanolic solution has the feature of strong fluorescent emission, before carrying out oxygenolysis, volatile oil fluorescence analysis method in rear Baizhu volatile oil/Benexate Hydrochloride, thus obtain the inclusion rate of inclusion compound, the indexs such as oil content, it is the valuable Baizhu volatile oil inclusion compound quality control method of a kind of science, the solution of this problem is expected to promote Baizhu volatile oil/Benexate Hydrochloride anti-cancer agent preparation R&D work.
Embodiment
embodiment 1
Instrument and condition:
VarianCaryEclipse fluorospectrophotometer, SK250H Ultrasound Instrument; KDC-1044 low speed centrifuge; FA-1004 analytical balance, GM-0.33 II vacuum diaphragm pump, β-CD, absolute ethyl alcohol, the volatile oil/Benexate Hydrochloride before oxygenolysis.
Emission wavelength: 429nm;
Excitation wavelength is respectively: 340nm, 367nm, 409nm;
Slit width is 5nm;
F
，=44.23C
，+9.30（1）
F
，，=（44.23C
，，+9.30）/B（2）。
Experimental procedure:
I. in inclusion compound, volatile oil ethanol takes off the preparation of bag solution:
Precision takes the volatile oil/Benexate Hydrochloride 30mg before oxygenolysis, adds 10mL absolute ethyl alcohol, ultrasonic 10min, refrigeration 24h; Subsequently with 2500r/min rotating speed, centrifugal 10min, gets supernatant liquor;
II. fluorescence analysis is carried out to supernatant liquor:
When excitation wavelength is 367nm, fluorescence analysis obtains its fluorescence intensity 31.136, and according to formula (1), in supernatant liquor, volatile oil content is 0.4937mg/mL, containing the volatile oil before the oxygenolysis of 4.937mg in 10mL volatile oil ethanolic solution, namely in inclusion compound, volatile oil content is 16.45%;
When excitation wavelength is 340nm, fluorescence analysis obtains its fluorescence intensity 6.742, B=31.136/6.742=4.62,
F
，，=（44.23C
，，+9.30）/B=9.57C
，，+2.01（2）
According to formula (2), in supernatant liquor, volatile oil content is that namely in inclusion compound, volatile oil content is 16.49% containing the volatile oil before the oxygenolysis of 4.947mg in 0.4947mg/mL, 10mL volatile oil ethanolic solution;
When excitation wavelength is 409nm, fluorescence analysis obtains its fluorescence intensity 16.755, B=31.136/16.755=1.87,
F
，，=（44.23C
，，+9.30）/B=23.65C
，，+4.97（2）
According to formula (2), in supernatant liquor, volatile oil content is that namely in inclusion compound, volatile oil content is 16.61% containing the volatile oil before the oxygenolysis of 4.983mg in 0.4983mg/mL, 10mL volatile oil ethanolic solution.
In inclusion compound, the mean value of volatile oil content is 16.51%, RSD=0.504%.
embodiment 2
Instrument and condition:
VarianCaryEclipse fluorospectrophotometer, SK250H Ultrasound Instrument; KDC-1044 low speed centrifuge; FA-1004 analytical balance, GM-0.33 II vacuum diaphragm pump, β-CD, absolute ethyl alcohol, the volatile oil/Benexate Hydrochloride after oxygenolysis.
Emission wavelength: 485nm;
Excitation wavelength is respectively: 315nm, 396nm, 465nm;
Slit width is 5nm;
F
，=38.68C
，+7.01（3）
F
，，=（38.68C
，，+7.01）/B（4）。
Experimental procedure:
I. in inclusion compound, volatile oil ethanol takes off the preparation of bag solution:
Precision takes the volatile oil/Benexate Hydrochloride 30mg after oxygenolysis, adds 10mL absolute ethyl alcohol, ultrasonic 10min, refrigeration 24h; Subsequently with 2500r/min rotating speed, centrifugal 10min, gets supernatant liquor;
II. fluorescence analysis is carried out to supernatant liquor:
When excitation wavelength is 396nm, fluorescence analysis obtains its fluorescence intensity 31.918, and according to formula (3), in supernatant liquor, volatile oil content is 0.6440mg/mL, containing the volatile oil after the oxygenolysis of 6.440mg in 10mL volatile oil ethanolic solution, namely in inclusion compound, volatile oil content is 21.46%;
When excitation wavelength is 315nm, fluorescence analysis obtains its fluorescence intensity 0.602, B=31.918/0.602=53.02,
F
，，=（38.68C
，，+7.01）/B=0.73C
，，+0.13（4）
According to formula (2), in supernatant liquor, volatile oil content is that namely in inclusion compound, volatile oil content is 21.55% containing the volatile oil before the oxygenolysis of 6.466mg in 0.6466mg/mL, 10mL volatile oil ethanolic solution;
When excitation wavelength is 465nm, fluorescence analysis obtains its fluorescence intensity 2.573, B=31.918/2.573=12.40,
F
，，=（38.68C
，，+7.01）/B=3.12C
，，+0.57（4）
According to formula (2), in supernatant liquor, volatile oil content is that namely in inclusion compound, volatile oil content is 21.40% containing the volatile oil before the oxygenolysis of 6.420mg in 0.6420mg/mL, 10mL volatile oil ethanolic solution.
In inclusion compound, the mean value of volatile oil content is 21.47%, RSD=0.352%.
Claims (1)
1. the assay method of volatile oil content in Baizhu volatile oil/Benexate Hydrochloride, it is characterized in that, described Baizhu volatile oil is the volatile oil before oxygenolysis or the volatile oil after oxygenolysis, volatile oil after described oxygenolysis is: the volatile oil before oxygenolysis is after oxygenolysis, and wherein the resolution ratio of atractylone reaches the Baizhu volatile oil of 100%;
The step of this assay method is:
I. in inclusion compound, volatile oil ethanol takes off the preparation of bag solution: precision takes Baizhu volatile oil/Benexate Hydrochloride, adds absolute ethyl alcohol, ultrasonic 10min, refrigeration 24h; Subsequently with 2500r/min rotating speed, centrifugal 10min, gets supernatant liquor; The mass volume ratio of inclusion compound and absolute ethyl alcohol is 3:1, and its unit is mg/ml;
II. fluorescence analysis is carried out to supernatant liquor:
If a. Baizhu volatile oil is the volatile oil before oxygenolysis, fluorescence condition is: take 429nm as emission wavelength, and with any wavelength within the scope of 340 ~ 409nm for excitation wavelength, slit width is 5nm, and fluorescence analysis obtains its fluorescence intensity F;
If 1. excitation wavelength is 367nm, its fluorescence intensity is F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (1)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，=44.23C
，+9.30（1）
In formula (1): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If 2. excitation wavelength is other wavelength, its fluorescence intensity is F
,, reduce multiple B=F
,/ F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (2)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，，=（44.23C
，，+9.30）/B（2）
In formula (2): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If b. Baizhu volatile oil is the volatile oil after oxygenolysis, fluorescence condition is: take 485nm as emission wavelength, and with any wavelength within the scope of 315 ~ 465nm for excitation wavelength, slit width is 5nm, and fluorescence analysis obtains its fluorescence intensity F;
If 1. excitation wavelength is 396nm, its fluorescence intensity is F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (3)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，=38.68C
，+7.01（3）
In formula (3): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor;
If 2. excitation wavelength is other wavelength, its fluorescence intensity is F
,, reduce multiple B=F
,/ F
,, try to achieve volatile oil content C in its supernatant liquor according to formula (4)
,, obtain volatile oil percentage composition in inclusion compound by calculating;
F
，，=（38.68C
，，+7.01）/B（4）
In formula (4): F
,for the fluorescence intensity of supernatant liquor;
C
,for the content (W/V) of volatile oil in supernatant liquor.
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|---|---|---|---|
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Citations (5)
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120043479A1 (en) * | 2010-08-17 | 2012-02-23 | Dow Agrosciences Llc. | Normalization of Biomolecules |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101825572A (en) * | 2010-06-11 | 2010-09-08 | 重庆大学 | Method for differentiating Chinese spirits with different flavor types with fluorescein |
| WO2013088883A1 (en) * | 2011-12-15 | 2013-06-20 | コニカミノルタ株式会社 | Device for chromatographic analysis and method for chromatographic analysis |
| CN102706844A (en) * | 2012-06-07 | 2012-10-03 | 苏州市中心血站 | Method for detecting content of methylene blue in blood plasma |
| CN103149187A (en) * | 2013-02-21 | 2013-06-12 | 江南大学 | Fluorescent method for rapidly determining content of aliphatic acid |
| CN103396890A (en) * | 2013-07-26 | 2013-11-20 | 山西省肿瘤医院 | Method for preparing stable bighead atractylodes rhizome volatile oil |
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| 香料-β -环糊精包合物的研究进展;孙建国;《枣庄学院学报》;20100430;第27卷(第2期);第48-51页 * |
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