CN105717238A - Method for detecting nuciferine in lotus leaf through liquid chromatography - Google Patents
Method for detecting nuciferine in lotus leaf through liquid chromatography Download PDFInfo
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- CN105717238A CN105717238A CN201610268726.2A CN201610268726A CN105717238A CN 105717238 A CN105717238 A CN 105717238A CN 201610268726 A CN201610268726 A CN 201610268726A CN 105717238 A CN105717238 A CN 105717238A
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- nuciferine
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- folium nelumbinis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention discloses a method for detecting nuciferine in a lotus leaf through liquid chromatography. The method comprises the following steps: 1) grinding the lotus leaf and sieving; 2) mixing lotus leaf powder with nano-silicon dioxide and then grinding; 3) mixing the mixture acquired from the step 2 with an extracting solvent; 4) putting container containing the mixture into an ultrasonic cleaner for extracting, thereby acquiring an extracting mixture; 5) filtering the extracting mixture and then diluting with the extraction agent, and performing liquid chromatography analysis on the diluted solution, thereby measuring the content of nuciferine. The invention provides the method for detecting nuciferine in the lotus leaf through liquid chromatography. According to the method, the nuciferine is extracted by adopting the ultrasonic extraction method and the nuciferine is detected by adopting the liquid chromatography; the detection precision is high; the difficulty in extraction and analysis operation is lowered.
Description
Technical field
The present invention relates to test in laboratory field, particularly a kind of by the method for nuciferine in liquid chromatography detection Folium Nelumbinis.
Background technology
Within 2015, pharmacopeia have recorded the extracting method of the nuciferine in Folium Nelumbinis: takes this product coarse powder and is about 0.5g, accurately weighed, puts in tool plug conical flask, accurate addition methanol 50ml, weighed weight, it is heated to reflux 2.5 hours, let cool, more weighed weight, the weight of less loss is supplied with methanol, shaking up, filter, precision measures subsequent filtrate 5ml, put in 10ml measuring bottle, add water to scale, shake up, to obtain final product.
Liquid chromatographic detection condition is: with octadecylsilane chemically bonded silica for filler；With acetonitrile one water one triethylamine glacial acetic acid (27:70.6:1.6:0.78) for mobile phase；Detection wavelength is 270nm.Number of theoretical plate calculates by nuciferine peak should be not less than 2000.
The method testing time of pharmacopeia, up to a few hours, extracts and detection process is complicated, use duration.
Summary of the invention
It is an object of the invention to provide a kind of by the method for nuciferine in liquid chromatography detection Folium Nelumbinis, the method adopts ultrasonic extraction method extraction nuciferine also to adopt liquid chromatography that nuciferine is detected, and accuracy of detection is high, and extraction and analysis operation difficulty is low.
Technical scheme provided by the invention is: a kind of by the method for nuciferine in liquid chromatography detection Folium Nelumbinis, comprises the following steps:
Step 1: after Folium Nelumbinis is pulverized, sieve,；
Step 2: grinding after being mixed with nano silicon by Folium Nelumbinis powder, the weight ratio of Folium Nelumbinis powder and nano silicon is 19:1；
Step 3: mixture step 2 obtained mixes with extractant, the ethanol that extractant is the acetic acid of 1 weight portion and the methanol of 4 weight portions and 5 weight portions mixes, and the weight ratio of mixture and extractant is 1:9；
Step 4: after the mixture of step 3 is heated to 50-55 DEG C, inserts the container accommodating mixture in ultrasonic cleaner and carries out extraction mixture is obtained by extraction；Extraction time is 30-35min；
Step 5: extracting after mixture filters of step 4 being obtained dilute with the extractant of the component described in step 3, easily will carry out liquid chromatography analysis after diluting, the content of mensuration nuciferine；
The parameter of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column C18Chromatographic column, 5 μm of 4.6 × 150mm
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water；The volume ratio of acetonitrile and water is 30:70
F) detection wavelength: 270nm.
Being detected in Folium Nelumbinis in the method for nuciferine by liquid chromatography above-mentioned, the supersonic frequency of described ultrasonic cleaner is 200KHz-300KHz
The present invention is after adopting technique scheme, and it has the beneficial effect that
The detection method of the present invention is simple to operate, and effect of extracting is consistent with the precision of official method, and reproducible, amount of samples is few, and extraction time is short.
In the present invention, Folium Nelumbinis adds nano silicon and can improve the effect of extracting in ultrasonic extraction process.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in further detail, but does not constitute any limitation of the invention.
Embodiment 1:
A kind of by the method for nuciferine in liquid chromatography detection Folium Nelumbinis, comprise the following steps:
Step 1: after Folium Nelumbinis is pulverized, sieve；
Step 2: grinding after being mixed with nano silicon by Folium Nelumbinis powder, the weight ratio of Folium Nelumbinis powder and nano silicon is 19:1；
Step 3: mixture step 2 obtained mixes with extractant, the ethanol that extractant is the acetic acid of 1 weight portion and the methanol of 4 weight portions and 5 weight portions mixes, and the weight ratio of mixture and extractant is 1:9；
Step 4: be heated to by the mixture of step 3: after 52 DEG C, inserts the container accommodating mixture in ultrasonic cleaner and carries out extraction mixture is obtained by extraction；Extraction time is 33min；Supersonic frequency is 250KHz.
Step 5: extracting of step 4 being obtained takes the extractant of the component described in 1ml step 3 after mixture filters and be diluted to 50ml, will easily carry out liquid chromatography analysis after dilution, measures the content of nuciferine；
The parameter of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column C18Chromatographic column, 5 μm of 4.6 × 150mm, i.e. carbon 18 chromatographic column, diameter 4.6mm, length 150mm, particle diameter 5 microns.
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water；The volume ratio of acetonitrile and water is 30:70
F) detection wavelength: 270nm.
The degree of accuracy test of the detection method of embodiment 1
Folium Nelumbinis is extracted and tests by the extraction and the detection method that adopt the ultrasonic extraction of embodiment 1 and detection method and pharmacopeia, and Folium Nelumbinis is 4 batches, lot number respectively 1512008,20150501,150820,1508144；Test result is shown in table 1 below:
Table 1
The above-described presently preferred embodiments of the present invention that is only, all any amendment, equivalent replacement and improvement etc. made within the scope of the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (2)
1. one kind is detected the method for nuciferine in Folium Nelumbinis by liquid chromatography, it is characterised in that comprise the following steps:
Step 1: after Folium Nelumbinis is pulverized, sieve；
Step 2: grinding after being mixed with nano silicon by Folium Nelumbinis powder, the weight ratio of Folium Nelumbinis powder and nano silicon is 19:1；
Step 3: mixture step 2 obtained mixes with extractant, the ethanol that extractant is the acetic acid of 1 weight portion and the methanol of 4 weight portions and 5 weight portions mixes, and the weight ratio of mixture and extractant is 1:9；
Step 4: after the mixture of step 3 is heated to 50-55 DEG C, inserts the container accommodating mixture in ultrasonic cleaner and carries out extraction mixture is obtained by extraction；Extraction time is 30-35min；
Step 5: extracting after mixture filters of step 4 being obtained dilute with the extractant of the component described in step 3, easily will carry out liquid chromatography analysis after diluting, the content of mensuration nuciferine；
The parameter of liquid chromatography is:
A) instrument: chromatograph of liquid
B) chromatographic column C18Chromatographic column, 5 μm of 4.6 × 150mm
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) mobile phase: acetonitrile-water；The volume ratio of acetonitrile and water is 30:70
F) detection wavelength: 270nm.
2. according to claim 1 by the method for nuciferine in liquid chromatography detection Folium Nelumbinis, it is characterised in that the supersonic frequency of described ultrasonic cleaner is 200KHz-300KHz.
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| CN201610268726.2A CN105717238A (en) | 2016-04-27 | 2016-04-27 | Method for detecting nuciferine in lotus leaf through liquid chromatography |
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| CN201610268726.2A CN105717238A (en) | 2016-04-27 | 2016-04-27 | Method for detecting nuciferine in lotus leaf through liquid chromatography |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680664A (en) * | 2018-04-28 | 2018-10-19 | 安徽粮食工程职业学院 | A kind of method of quick measurement Nuciferine purity |
| CN108918735A (en) * | 2018-07-31 | 2018-11-30 | 四川新绿色药业科技发展有限公司 | A kind of efficient liquid phase method detecting lotus leaf medicinal material, medicine materical crude slice, standard decoction, granule characteristic spectrum |
| CN110658295A (en) * | 2019-10-23 | 2020-01-07 | 葵花药业集团（襄阳）隆中有限公司 | Method for measuring fingerprint spectrum of lotus leaf decoction pieces in Erdong decoction formula |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085041A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Total alkaloid of lotus leaves extraction and its preparation method |
| CN101139320A (en) * | 2007-09-01 | 2008-03-12 | 福州大学 | Method for separating nuciferine and lotus leaf flavone from lotus leaf |
| CN102442949A (en) * | 2010-10-09 | 2012-05-09 | 苏州宝泽堂医药科技有限公司 | Method for extracting nuciferine from lotus leaves |
-
2016
- 2016-04-27 CN CN201610268726.2A patent/CN105717238A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085041A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Total alkaloid of lotus leaves extraction and its preparation method |
| CN101139320A (en) * | 2007-09-01 | 2008-03-12 | 福州大学 | Method for separating nuciferine and lotus leaf flavone from lotus leaf |
| CN102442949A (en) * | 2010-10-09 | 2012-05-09 | 苏州宝泽堂医药科技有限公司 | Method for extracting nuciferine from lotus leaves |
Non-Patent Citations (3)
| Title |
|---|
| 唐伯辰 等: "HPLC测定不同生长期和采收期太空莲叶中荷叶碱的含量", 《湖南中医药大学学报》 * |
| 郑振佳: "超声辅助提取-高效液相色谱法测定荷叶中的生物碱", 《食品与发酵工业》 * |
| 陈凌 等: "荷叶中荷叶碱的高效液相色谱检测方法及其提取工艺研究", 《食品与机械》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680664A (en) * | 2018-04-28 | 2018-10-19 | 安徽粮食工程职业学院 | A kind of method of quick measurement Nuciferine purity |
| CN108918735A (en) * | 2018-07-31 | 2018-11-30 | 四川新绿色药业科技发展有限公司 | A kind of efficient liquid phase method detecting lotus leaf medicinal material, medicine materical crude slice, standard decoction, granule characteristic spectrum |
| CN108918735B (en) * | 2018-07-31 | 2021-06-22 | 四川新绿色药业科技发展有限公司 | High performance liquid chromatography method for detecting characteristic spectrums of lotus leaf medicinal materials, decoction pieces, standard decoction and formula granules |
| CN110658295A (en) * | 2019-10-23 | 2020-01-07 | 葵花药业集团（襄阳）隆中有限公司 | Method for measuring fingerprint spectrum of lotus leaf decoction pieces in Erdong decoction formula |
| CN110658295B (en) * | 2019-10-23 | 2022-02-25 | 葵花药业集团（襄阳）隆中有限公司 | Method for measuring fingerprint spectrum of lotus leaf decoction pieces in Erdong decoction formula |
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