CN102818862B - Method for simultaneously determining content of three components for traditional Chinese medicine phyllanthus emblica through whole-time three-wavelength fusion - Google Patents
Method for simultaneously determining content of three components for traditional Chinese medicine phyllanthus emblica through whole-time three-wavelength fusion Download PDFInfo
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Abstract
The invention discloses a method for simultaneously determining content of three components for traditional Chinese medicine phyllanthus emblica through whole-time three-wavelength fusion. According to the method, a modern analysis detection method and an information processing method are combined, spectrogram information of marker components of Chinese herbal medicines is effectively fused, determined components are the largest ultraviolet absorption wavelengths, the signal to noise ratio of the determined components is increased, the defect of insufficient information amount of single wavelength and index detection can be overcome, and internal quality of Chinese herbal medicines can be reflected perfectly. The quality control method of the three components is simple in operation, stable and reliable, good in reproducibility, and capable of being applied to quality evaluation and control of Chinese herbal medicines and new drug development, particularly serving as one of indexes of quality control and identification for the traditional Chinese medicine phyllanthus emblica.
Description
Invention field
The invention belongs to the technical field that adopts modern analysis detection means and information processing means to detect the quality of Chinese crude drug, the content control method that relates to a kind of Chinese crude drug multi-target ingredient, says that a kind of Chinese medicine emblic all the period of time three-wavelength merges the method for simultaneously measuring three kinds of component contents more specifically.
Background technology
According to record of Pharmacopoeia of People's Republic of China version in 2010: this product is the dry mature fruit of euphorbia plant emblic Phyllanthus emblica L., winter to the spring gathers during fruit maturation, removes impurity, dry.Emblic begins to be loaded in < < south vegetation shape > >.Emblic taste is sweet, cold, nontoxic, for heat-clearing pyogenic infections, and relieve sore throat moistening lung, preventing phlegm from forming and stopping coughing, promotes the production of body fluid to quench thirst.Emblic cures mainly that blood disease, red bar are sick, Baconic is sick, hepatopathy, and heart disease and high blood pressure, take and treat blood disease that blood-head blood stasis causes as long.Research in recent years shows that emblic has the effects such as anti-oxidant, anticancer, antiviral, reducing blood lipid.Emblic main product is in Yunnan, Sichuan, Guangdong, Guangxi.Emblic mainly contains tannin class, flavonoids, polysaccharide and vitamin C, and tannin class is mainly gallic acid, chebulinic acid, Chebulagic acid, Chebulic acid, ellagic acid, epicatechin etc.; Flavonoids is mainly Quercetin, Kaempferol, rutin etc.; Polysaccharide is D-Glucose, D-Fructose, sucrose etc.
Along with scientific and technical development, the generally use of modern advanced analysis detecting instrument and the gradual perfection of the information processing technology, had Analysis of Chinese Traditional Medicine detection level and significantly improve, and traditional Chinese medicine quality control method is updated.By setting up HPLC collection of illustrative plates, Chinese crude drug index components is carried out to a kind of development trend that assay becomes traditional Chinese medicine quality control and evaluates in recent years.Chinese medicine HPLC collection of illustrative plates refers to that some Chinese crude drug or Chinese patent drug are after suitable processing, spectrogram or the chromatogram that can manifest Chinese crude drug or pcm chemical feature that utilize present information acquisition technique and quality analysis means to obtain.Due under three different chromatographic conditions, use different pre-treating methods to emblic in gallic acid, epicatechin and ellagic acid detect respectively to realize emblic medicinal material carried out comprehensively and the overall evaluation, therefore, follow information maximization principle and set up all the period of time three-wavelength and merge and to measure three kinds of index components content of Chinese medicine emblic simultaneously and can obtain a kind of comparatively effectively method of quality control, thereby guarantee the safe, stable and reliable of emblic quality of medicinal material.
Emblic medicinal material occupies very consequence in Chinese crude drug.At present, commercially available emblic quality of medicinal material is uneven, so the stability of emblic medicinal material is difficult to guarantee.The assay of 2010 editions Chinese Pharmacopoeia regulations: this product is pressed dry product and calculated, containing gallic acid (C
7h
6o
5) must not be less than 1.2%.
Summary of the invention
The object of the invention is to adopt modern analysis detection means and information processing means to set up emblic medicinal material all the period of time three-wavelength fusion HPLC graphical spectrum technology, and the content assaying method of three index components wherein, easier, reasonable, reliable to guarantee the method for quality control of emblic medicinal material.
The present invention is achieved by the following technical solutions:
Chinese medicine emblic all the period of time three-wavelength merges the method for simultaneously measuring three kinds of component contents, it is characterized in that comprising lower step:
(1) preparation of need testing solution: get the about 3-5g of emblic medicinal material (crossing 16 mesh sieves), accurately weighed, put in round-bottomed flask, precision adds 70% ethanol 33mL, add hot reflux 1-2 hour, extract three times, reclaim merging filtrate, add water and be settled to 20ml, making solution final concentration is 0.15g/ml, the accurate subsequent filtrate 17mL that draws, be added on polyamide resin column, with distilled water 90mL, wash, use again 105mL 50% ethanol elution, collect ethanol eluate, evaporate to dryness, residue adds methyl alcohol to be made to dissolve and is transferred in 10mL measuring bottle, add methanol constant volume to scale, shake up, filter, get subsequent filtrate, obtain,
(2) preparation of reference substance solution: it is appropriate that precision takes gallic acid reference substance, epicatechin reference substance, ellagic acid reference substance and Quercetin reference substance, add methyl alcohol and make respectively every 1mL containing gallic acid reference substance 0.44mg, epicatechin reference substance 0.1495mg and ellagic acid reference substance 0.03775mg, obtain;
(3) chromatographic condition and system suitability: the Agilent TC-C18 that is filling agent with octadecyl silane (4.6mm * 250 mm, 5 μ m) chromatographic column; Take 0.2% phosphoric acid water as mobile phase A, take acetonitrile as Mobile phase B, carry out gradient elution; Flow velocity 1.0mL/min; 35 ℃ of column temperatures; DAD detecting device detects under wavelength 230nm, 254nm and 280nm simultaneously; Sample size 5 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
(4) all the period of time three-wavelength fusion: adopt multi-wavelength fusion HPLC graphical spectrum technology that the spectral data under 230nm, 254nm and tri-wavelength of 280nm is carried out to all the period of time fusion, obtain a chromatic graph spectrum that can simultaneously comprise three wavelength information.
(5) sample size is measured: the HPLC spectrum data after application is merged, the content of three kinds of index components in calculation sample.
(6) above-mentioned definite content assaying method is carried out to efficiency evaluation, comprising specificity, accuracy, precision, repeatability, stability, the range of linearity and durability.
Chinese medicine emblic all the period of time three-wavelength of the present invention merges the method for simultaneously measuring three kinds of component contents to be compared had good effect with the assay method of existing Chinese Pharmacopoeia regulation and is:
(1) method that the present invention is openly merged HPLC collection of illustrative plates and its index components carried out to assay by setting up emblic medicinal material all the period of time three-wavelength first, the method is to same sample heterogeneity multi-wavelength Simultaneous Quantitative Analysis, thus perfect emblic quality of medicinal material control method.
(2) the present invention adopts modern advanced analysis detection technique, and three index components of emblic medicinal material are carried out to analyzing and testing, thereby obtains extremely abundant quantity of information.
(3) the present invention carries out all the period of time fusion by information processing means by the chromatogram under emblic medicinal material three-wavelength, is guaranteeing, under the prerequisite of data message loss reduction, to obtain the chromatogram of three wavelength information of a simultaneous reactions.
(4) three kinds of index components content control methods of the present invention, its advantage is simple to operate, reliable and stable, precision, repeatability, the recovery all reach quantitative test requirement, can comprehensively analyze on a macro scale the quality of emblic medicinal material.
(5) the present invention is merged HPLC collection of illustrative plates by setting up emblic medicinal material all the period of time three-wavelength, the element of the second species in emblic medicinal material is carried out to qualitative and quantitative analysis, disclose truly the inherent quality feature of emblic medicinal material comprehensively, thereby guaranteed the safe, effective, reliable, stable of emblic medicinal material, guaranteed the equalization stable of its quality and the standardization of technique.
Accompanying drawing explanation
Fig. 1 is the HPLC chromatogram of reference substance gallic acid, epicatechin and ellagic acid under 230nm wavelength.
Fig. 2 is the HPLC chromatogram of reference substance gallic acid, epicatechin and ellagic acid under 254nm wavelength.
Fig. 3 is the HPLC chromatogram of reference substance gallic acid, epicatechin and ellagic acid under 280nm wavelength.
Fig. 4 is the UV scanning figure of gallic acid.
Fig. 5 is the UV scanning figure of epicatechin.
Fig. 6 is the UV scanning figure of ellagic acid.
Fig. 7 is HPLC chromatogram under emblic medicinal material 230nm wavelength.
Fig. 8 is HPLC chromatogram under emblic medicinal material 254nm wavelength.
Fig. 9 is HPLC chromatogram under emblic medicinal material 280nm wavelength.
Figure 10 is the chromatogram of emblic medicinal material all the period of time multi-wavelength fusion.
Embodiment
Chinese medicine emblic all the period of time three-wavelength merges the method for simultaneously measuring three kinds of component contents, comprises the steps:
1, the preparation of need testing solution:
Get emblic medicinal material (crossing 16 mesh sieves) 3g, accurately weighed, put in round-bottomed flask, precision adds 70% ethanol 33mL, add hot reflux 1.5 hours, extract three times, reclaim merging filtrate, add water and be settled to 20ml, making solution final concentration is 0.15g/ml, and the accurate subsequent filtrate 17mL that draws, is added on polyamide resin column, with distilled water 90mL, wash, use again 105mL 50% ethanol elution, collect ethanol eluate, evaporate to dryness, residue adds methyl alcohol to be made to dissolve and is transferred in 10mL measuring bottle, add methanol constant volume to scale, shake up, filter, get subsequent filtrate, obtain;
2, chromatographic condition and compatibility test: the Agilent TC-C18 that is filling agent with octadecyl silane (4.6mm * 250 mm, 5 μ m) chromatographic column; Take 0.2% phosphoric acid water as mobile phase A, take acetonitrile as Mobile phase B, carry out gradient elution, flow velocity 1.0mL/min; 35 ℃ of column temperatures; DAD detecting device detects under wavelength 230nm, 254nm and 280nm simultaneously; Sample size 5 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
Table 1 eluent gradient wash-out table
3 kinds of component content control methods of emblic medicinal material of the present invention, by analysis and detecting instrument, obtain the spectral data under 230nm, 254nm, tri-wavelength of 280nm, exploit information is processed the spectral data under three wavelength of means all the period of time fusion, obtains a chromatic graph spectrum that can simultaneously comprise three wavelength information.
3 kinds of component content control methods of emblic medicinal material of the present invention, by 230nm, 254nm, 280nm
After spectral data all the period of time fusion under three wavelength, can obtain one group of spectral data.Wherein finger-print data are in Table 2
Table 2 merges peak spectrum data
| Peak order | Retention time | Peak height | Peak |
| 1 | 10.554 | 309.1344 | 7051.687 |
| 2 | 36.494 | 137.2737 | 3011.118 |
| 3 | 54.50067 | 117.2189 | 1999.186 |
Emblic quality of medicinal material control method of the present invention, the HPLC spectrum data obtaining, can be for the quantitative test of emblic medicinal material index components.
Claims (1)
1. Chinese medicine emblic all the period of time three-wavelength merges the method for simultaneously measuring three kinds of component contents, it is characterized in that comprising the steps:
(1) preparation of need testing solution: get emblic medicinal material, cross 16 mesh sieves, about 3g, accurately weighed, put in round-bottomed flask, precision adds 70% ethanol 33mL, add hot reflux 1.5 hours, extract three times, reclaim merging filtrate, add water and be settled to 20ml, making solution final concentration is 0.15g/ml, the accurate subsequent filtrate 17mL that draws, be added on polyamide resin column, with distilled water 90mL, wash, use again 105mL50% ethanol elution, collect ethanol eluate, evaporate to dryness, residue adds methyl alcohol to be made to dissolve and is transferred in 10mL measuring bottle, add methanol constant volume to scale, shake up, filter, get subsequent filtrate, obtain,
(2) preparation of reference substance solution: it is appropriate that precision takes gallic acid reference substance, epicatechin reference substance and ellagic acid reference substance, add methyl alcohol and make respectively every 1mL containing gallic acid reference substance 0.44mg, epicatechin reference substance 0.1495mg and ellagic acid reference substance 0.03775mg, obtain;
(3) chromatographic condition and system suitability: the Agilent TC-C18 chromatographic column that is filling agent with octadecyl silane; Chromatographic column specification is: 4.6mm * 250mm, 5 μ m; Take 0.2% phosphoric acid water as mobile phase A, and the acetonitrile of take carries out gradient elution as Mobile phase B; Flow velocity 1.0mL/min; 35 ℃ of column temperatures; DAD detecting device detects under wavelength 230nm, 254nm and 280nm simultaneously; Sample size 5 μ L; Theoretical cam curve is calculated, and should be not less than 3000;
Eluent gradient elution technique parameter is:
(4) all the period of time three-wavelength fusion: adopt multi-wavelength fusion technology to carry out all the period of time fusion to the spectral data under 230nm, 254nm and tri-wavelength of 280nm, obtain a chromatogram that can simultaneously comprise three wavelength information;
(5) sample size is measured: the HPLC spectrum data after application is merged, the content of three kinds of index components in calculation sample;
(6) above-mentioned definite content assaying method is carried out to efficiency evaluation, comprising specificity, accuracy, precision, repeatability, stability, the range of linearity and durability.
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| Identification of phenolics in the fruit of emblica (Phyllanthus emblica L.) and their antioxidant activities;Xiaoli Liu等;《Food Chemistry》;20080815;第109卷(第4期);第909–915页 * |
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| 余甘子总酚酸和总黄酮配伍抑制肝癌细胞增殖及对免疫功能的调节作用;朱英环等;《中国实验方剂学杂志》;20120229;第18卷(第3期);第132-135页 * |
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