CN104020235B - A kind of method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content - Google Patents
A kind of method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content Download PDFInfo
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Abstract
The invention provides a kind of method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content, it comprises ultrasonic wave extraction and quantitative analysis etc., when ultrasonic wave extracts, the solid-to-liquid ratio of Honeysuckle Flower and 70% ethanol water is 1: 80-1: 120, and extraction time 45-60min. Does is UPLC condition: chromatographic column: Waters? Acquity? UPLC? BEH? RP18; Mobile phase: acetonitrile-0.4% phosphoric acid water; Gradient elution: 0-2min, 5%-16%B; 2-4min, 16%-20%B; 4-8min, 20%-50%B; 8-10min, 50%-100%B; 10-11min, 100%-5%B; Detect wavelength: 242nm. The inventive method is simple, can measure the content of Chlorogenic Acid of Flos Lonicerae and galuteolin simultaneously, and highly sensitive, preci-sion and accuracy is high, reproducible, reliable and stable.
Description
Technical field
The present invention relates to the detection method of effective ingredient of honeysuckle, relating more specifically to one can be simultaneously rightActive ingredient-chlorogenic acid of honeysuckle and galuteolin carry out the method for quantitative analysis.
Background technology
Honeysuckle is that dry flower or the band of caprifoliaceae plant honeysuckle LonicerajaponicaThunb. just openedFlower, traditional Chinese medicine, has effect of clearing heat and detoxicating, dispelling wind and heat from the body, antiviral, hepatic cholagogic. GoldHoneysuckle flower main product is in the ground such as Henan, Shandong, its main chemical compositions be organic acid, triterpenes, flavonoids andVolatilization wet goods, wherein Determination of Organic Acids is antibacterial, the antiviral active component of honeysuckle. Chlorogenic acid is goldOne of main active ingredient of honeysuckle flower, not only as the quality control index of its crude drug, is also some one-tenthThe quality control index of medicine and preparation. In 2010 editions pharmacopeia taking chlorogenic acid and galuteolin as index compositionHoneysuckle is carried out to quality control.
At present technology and the means of chlorogenic acid and galuteolin quantitative analysis are mainly contained: thin layer chromatography scanning(TLCS), capillary electrophoresis (CE), high performance liquid chromatography (HPLC), liquid-matter GC-MS(LC-MS) etc., wherein universal with HPLC method. Ultra Performance Liquid Chromatography method (UPLC) is adoptedBy granule filler chromatographic column, (particle diameter is generally less than 2 μ m) and super-pressure (pressure is greater than 105KPa)A kind of isolation technics of system, with respect to HPLC, it more can significantly improve separating degree and the inspection of chromatographic peakSurvey sensitivity, simultaneously can shorten analysis time, reduce the use etc. of organic reagent, extensively should at presentFor the constituent analysis of Chinese herbal medicine. UPLC has been reported in the quantitative analysis of Chlorogenic Acid of Flos Lonicerae,But how quick, measure exactly the side of Chlorogenic Acid of Flos Lonicerae and two kinds of component contents of galuteolin simultaneouslyMethod need research.
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of accurately, fast and can measure gold simultaneouslyThe method of the content of honeysuckle flower Content of Chlorogenic Acid and galuteolin.
The method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention, comprises followingStep:
Ultrasonic wave extracts: extracting honeysuckle powder sieves, according to 1: 80-1: 120 solid-to-liquid ratio, adds 70%Ethanol water, weighed weight, ultrasonic extraction 45-60min, lets cool, and obtains Flos Lonicerae extractive solution.
Quantitative analysis: utilize UPLC-PDA method to carry out quantitative analysis, wherein UPLC condition: chromatogramPost is WatersAcquityUPLCBEHRP18(100mm × 2.1mmi.d., 1.7 μ are m); Room temperature,Mobile phase: A:B=0.4% phosphoric acid water: acetonitrile; Condition of gradient elution: equilibration time is 5min; GradientElution program: 0～2min, 5%～16%B; 2～4min, 16%～20%B; 4～8min, 20%～50%B; 8～10min, 50%～100%B; 10～11min, 100%～5%B; Sample size: 3 μ L, detectWavelength: 242nm, volume flow 0.2mL/min.
Preferably, in ultrasonic wave extraction step, Honeysuckle Flower, according to the solid-to-liquid ratio of 1: 120, adds 70%Ethanol water, weighed weight, ultrasonic extraction 45min, lets cool, and obtains Flos Lonicerae extractive solution.
Preferably, in quantitative analysis step, also comprise: the preparation of reference substance solution: precision takes green formerAcid, galuteolin reference substance: 0.889mg, 0.920mg, taking acetonitrile-0.4% phosphate aqueous solution as solvent,In brown volumetric flask, be settled to 2mL, as storing solution. The reference substance solution of other different quality concentrationObtained by storing solution dilution.
Preferably, in ultrasonic wave extraction step, Honeysuckle Flower is crossed 65-80 mesh sieve.
Preferably, before quantitative analysis, carry out the preparation of need testing solution, comprising: extracting honeysuckle extractsLiquid is supplied weight with 70% ethanol water, shakes up, and filters, and crosses 0.22 μ m miillpore filter, obtains confessionTest sample solution.
The method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention, method is simple,Can measure the content of Chlorogenic Acid of Flos Lonicerae and galuteolin simultaneously, have highly sensitive, precision andThe degree of accuracy is high, reproducible, reliable and stable advantage.
1, method is simple, and the time is short, adopts ultrasonic wave to extract in the present invention, and simple to operate, efficiency is high,In described ultrasonic wave extraction step, select 70% ethanol water greatly to improve extraction efficiency, shortenedExtraction time, inventor studies discovery, selects 70% ethanol water as extracting solvent, when extractionBetween only need 45min, greatly shortened extraction time.
2, extraction efficiency is high, and testing result is accurate, in ultrasonic wave extraction step, Honeysuckle Flower according toThe solid-to-liquid ratio of 1: 120, adds 70% ethanol water, weighed weight. Inventor studies discovery, works as gold and silverThe solid-to-liquid ratio of pollen end and 70% ethanol water is lower than 1: 120 o'clock, Flos Lonicerae extractive solution Content of Chlorogenic AcidHave overload phenomenon, when the solid-to-liquid ratio of the ethanol water of Honeysuckle Flower and 70% is during higher than 1: 120,The response of galuteolin is lower, affects testing result.
3, the method for simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention, utilizes superHigh performance liquid chromatography (UPLC), Ultra Performance Liquid Chromatography method (UPLC) is to adopt granule filler look(particle diameter is generally less than 2 μ m) and the one of super-pressure (pressure is greater than 105KPa) system is divided for spectrum postFrom technology, with respect to HPLC, it more can significantly improve separating degree and the detection sensitivity of chromatographic peak, withIn time, can shorten analysis time, reduces the use etc. of organic reagent.
4, the present invention utilizes UPLC-PDA method to measure Chlorogenic Acid of Flos Lonicerae and galuteolin simultaneouslyContent, its chromatographic condition adopting can be realized within shorter analysis time, and two kinds of materials are reachedGood separation. When gradient elution, the chromatogram baseline that the phosphate aqueous solution of mobile phase employing 0.4% obtains is flatSurely, and the separating degree of chlorogenic acid and galuteolin good; Use RP18 post separating effect better; Work as rippleLong during for 242nm, its response can accurate response chlorogenic acid and the content of galuteolin.
The method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention can be measured simultaneouslyThe content of Chlorogenic Acid of Flos Lonicerae and galuteolin, method accurately, fast, be the quality control of honeysuckleReliable evaluation method is provided.
Brief description of the drawings
Fig. 1 be the method for simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention whereinThe UPLC-PDA chromatogram of sample and reference substance.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail, to make those skilled in the art's referenceDescription word can be implemented according to this.
The method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content of the present invention, comprises followingStep:
Ultrasonic wave extracts: extracting honeysuckle powder sieves, according to 1: 80-1: 120 solid-to-liquid ratio, adds 70%Ethanol water, weighed weight, ultrasonic extraction 45-60min, lets cool, and obtains Flos Lonicerae extractive solution.
Quantitative analysis: extracting honeysuckle extract is supplied weight with 70% ethanol water, shakes up, filters,Cross 0.22 μ m miillpore filter, obtain need testing solution;
UPLC condition: chromatographic column is WatersAcquityUPLCBEHRP18(100mm×2.1mmI.d., 1.7 μ m); Room temperature, mobile phase: A:B=0.4% phosphoric acid water: acetonitrile; Condition of gradient elution: flatThe weighing apparatus time is 5min; Gradient elution program: 0～2min, 5%～16%B; 2～4min, 16%～20%B;4～8min，20％～50％B；8～10min，50％～100％B；10～11min，100％～5％B；Sample size: 3 μ L, detect wavelength: 242nm, volume flow 0.2mL/min.
Wherein, in ultrasonic wave extraction step, Honeysuckle Flower is according to the solid-to-liquid ratio of 1: 120, adds 70%Ethanol water, weighed weight, ultrasonic extraction 45min, lets cool, and obtains Flos Lonicerae extractive solution.
Wherein, in quantitative analysis step, also comprise: the preparation of reference substance solution: precision takes chlorogenic acid,Galuteolin reference substance: 0.889mg, 0.920mg, taking acetonitrile-0.4% phosphate aqueous solution as solvent, inIn brown volumetric flask, be settled to 2mL, as storing solution. The reference substance solution of other different quality concentration byStoring solution dilution obtains.
Wherein, in ultrasonic wave extraction step, Honeysuckle Flower is crossed 65-80 mesh sieve.
Embodiment 1
The method of the content of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin of the present invention, employingInstrument and material:
WatersAcquityUPLCH-Class system, comprises quaternary pump, the online degasser of vacuum, automaticallyInjector, PDA detector, Empower work station. 100000/balance (Mei Tele company);EL204 ten thousand/balance (Shanghai precision instrument Co., Ltd); KQ-250DE ultrasonic cleaner (elder brotherUltrasonic instrument Co., Ltd of mountain city).
Methyl alcohol and acetonitrile (chromatographically pure, Fisher company), ethanol, phosphoric acid (analyze pure, Beijing Chemical Plant),Distilled water. Reference substance chlorogenic acid (NO:110753-201314) and galuteolin (NO:111720-201106)Purchased from National Institute for Food and Drugs Control. Honeysuckle material source is in table 3, through Medicinal Plants of Guangxi gardenWu Qinghua assistant researcher is accredited as the dried floral of caprifoliaceae plant honeysuckle LonicerajaponicaThunb.Flower bud.
The method of the content of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin of the present invention, comprise withLower step:
(1) preparation of reference substance solution: precision takes chlorogenic acid, galuteolin reference substance: 0.889mg,0.920mg taking acetonitrile-0.4% phosphate aqueous solution as solvent, is settled to 2mL in brown volumetric flask, doesFor storing solution. The reference substance solution of other different quality concentration is obtained by storing solution dilution.
(2) preparation of need testing solution: the about 0.25g of extracting honeysuckle powder (crossing 60 mesh sieves), precisionWeighed, be placed in tool plug conical flask, precision adds 70% ethanol water 25mL, and weighed weight is superSound extracts (power 250W, frequency 40HZ) 45min, lets cool, and supplies with 70% ethanol waterThe weight reducing, shakes up, and filters, and gets subsequent filtrate appropriate, crosses 0.22 μ m miillpore filter, to obtain final product.
(3) chromatographic condition: chromatographic column is WatersAcquityUPLCBEHRP18(100mm×2.1Mmi.d., 1.7 μ m); Room temperature, mobile phase is 0.4% phosphoric acid water (A)-acetonitrile (B), gradient elution,Equilibration time is 5min, gradient elution program: 0～2min, 5%～16%B; 2～4min, 16%～20%B；4～8min，20％～50％B；8～10min，50％～100％B；10～11min，100％～5％B；Sample size: 3 μ L, detect wavelength: 242nm, volume flow 0.2mL/min.
(4) sample determination
Get respectively the traditional Chinese medicine honeysuckle powder in 10 batches of different places of production, utilize the gold of simultaneously measuring of the present inventionThe method of the content of honeysuckle flower Content of Chlorogenic Acid and galuteolin, and adopt external standard method to calculate, the results are shown in Table 1.
The traditional Chinese medicine honeysuckle Content of Chlorogenic Acid in the table 110 batch different places of production and the assay result of galuteolin
As shown in Table 1, utilize Chlorogenic Acid of Flos Lonicerae and the galuteolin content simultaneously measured of the present inventionMethod, the content of the Chlorogenic Acid of Flos Lonicerae of surveying and galuteolin accurate, data are reliable.
As shown in Figure 1, from the UPLC-PDA chromatogram of sample 7 and reference substance, can find out gold and silverThe crest of flower Content of Chlorogenic Acid 1 and galuteolin 2 is clear, and good separating effect, is convenient to survey rapidly and accuratelyAmount.
Embodiment 2
The method of the content of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin of the present invention, comprise withLower step:
(1) preparation of reference substance solution: precision takes chlorogenic acid, galuteolin reference substance: 0.889mg,0.920mg taking acetonitrile-0.4% phosphate aqueous solution as solvent, is settled to 2mL in brown volumetric flask, doesFor storing solution. The reference substance solution of other different quality concentration is obtained by storing solution dilution.
(2) preparation of need testing solution: the about 0.25g of extracting honeysuckle powder (crossing 60 mesh sieves), precisionWeighed, be placed in tool plug conical flask, precision adds 70% ethanol water 30mL, and weighed weight is superSound extracts (power 250W, frequency 40HZ) 45min, lets cool, and supplies with 70% ethanol waterThe weight reducing, shakes up, and filters, and gets subsequent filtrate appropriate, crosses 0.22 μ m miillpore filter, to obtain final product.
(3) chromatographic condition: chromatographic column is WatersAcquityUPLCBEHRP18(100mm×2.1Mmi.d., 1.7 μ m); Room temperature, mobile phase is: 0.4% phosphoric acid water (A)-acetonitrile (B), gradient is washedDe-, equilibration time is 5min, gradient elution program: 0～2min, 5%～16%B; 2～4min, 16%～20%B；4～8min，20％～50％B；8～10min，50％～100％B；10～11min，100％～5％B；Sample size: 3 μ L, detect wavelength: 242nm, volume flow 0.2mL/min.
(4) foundation of calibration curve
A, the investigation of linear relationship, detectability (LOD) and quantitative limit (LOQ)
The respectively accurate reference substance storing solution of drawing, becomes the right of a series of variable concentrations with mobile phase stepwise dilutionAccording to product solution, sample introduction 3 μ L respectively, measure (n=3). Chlorogenic acid and galuteolin are taking concentration X as horizontalCoordinate, average peak area Y is that ordinate carries out linear regression, investigates linear relationship. Get mixing reference substanceStoring solution is appropriate, adds mobile phase stepwise dilution, and under above-mentioned chromatographic condition, sample introduction is measured, and signal to noise ratio is 3: 1Be respectively detectability (LOD) and the quantitative limit (LOQ) of chlorogenic acid and galuteolin with the concentration of 10: 1 o'clock.As shown in Table 2, each regression equation is good linear relationship.
Calibration curve, coefficient correlation, the range of linearity, LOD and the LOQ of table 2 chlorogenic acid and galuteolinMeasurement result
B, precision, repeatability and stability test
The accurate reference substance mixed liquor 3 μ L that draw, under above-mentioned chromatographic condition, continuous sample introduction 6 times, records greenThe RSD value of ortho acid and galuteolin is respectively: 0.85%, 1.04%, and result shows that the precision of instrument is goodGood. Get with the about 0.25g of a collection of Honeysuckle Flower, totally 6 parts, accurately weighed, by test sample preparation methodMake need testing solution, under above-mentioned chromatographic condition, measure, the average content that records chlorogenic acid is34.86mg/g, RSD is 1.17%; The average content of galuteolin is 1.24mg/g, and RSD is 1.28%,Result shows that this method repeatability is good. Get with a collection of Honeysuckle Flower (No: 7 Qufu City, Shandong Provinces) test sample moltenLiquid, places under room temperature, respectively at 0,2,4,8,16,24h sample introduction, 3 μ L, by above-mentioned chromatostripPart is measured, and records peak area, the RSD value of chlorogenic acid and galuteolin peak area is respectively 1.64%,1.59%, result shows that need testing solution is stable in 24h.
C, recovery test
Adopt application of sample absorption method. Get 9 parts of the Honeysuckle Flowers of known content, every part of about 0.125g, precisionWeighed, be divided into 3 groups, by low (80%), in (100%), high (120%) concentration respectively precision addsA certain amount of chlorogenic acid and galuteolin reference substance solution, according to preparation method's preparation of test sample, upperState chromatographic condition and measure, calculate recovery rate. Result demonstration, the rate of recovery reaches more than 97% entirely, seesTable 3. Result confirms that the method for setting up is for measure containing of Chlorogenic Acid of Flos Lonicerae and galuteolin simultaneouslyMeasurer has the higher degree of accuracy.
Table 3 application of sample recovery test result (n=9)
Although embodiment of the present invention are open as above, it is not restricted to description and enforcement sideListed utilization in formula, it can be applied to various applicable the field of the invention completely, for being familiar with abilityThe personnel in territory, can easily realize other amendment, therefore do not deviate from claim and etc. homotypeEnclose under limited universal, the present invention is not limited to specific details and illustrates here and the figure describingExample.
Claims (3)
1. a method of simultaneously measuring Chlorogenic Acid of Flos Lonicerae and galuteolin content, is characterized in that,Can carry out quantitative analysis to Chlorogenic Acid of Flos Lonicerae and galuteolin, it comprises the following steps simultaneously:
Ultrasonic wave extracts: extracting honeysuckle powder sieves, and according to the solid-to-liquid ratio of 1:80-1:120, adds 70%Ethanol water, weighed weight, ultrasonic extraction 45-60min, lets cool, and obtains Flos Lonicerae extractive solution;
Quantitative analysis: utilize UPLC-PDA method to carry out quantitative analysis, wherein UPLC condition: chromatogramPost is WatersAcquityUPLCBEHRP18, its specification is 100mm × 2.1mmi.d., 1.7 μ m;Room temperature, mobile phase: A:B=0.4% phosphoric acid water: acetonitrile; Condition of gradient elution: equilibration time is 5min;Gradient elution program: 0～2min, 5%～16%B; 2～4min, 16%～20%B; 4～8min, 20%～50%B; 8～10min, 50%～100%B; 10～11min, 100%～5%B; Sample size: 3 μ L, detectWavelength: 242nm, volume flow 0.2mL/min; In quantitative analysis step, also comprise: reference substance is moltenThe preparation of liquid: precision takes chlorogenic acid, galuteolin reference substance: 0.889mg, 0.920mg, with acetonitrile-0.4% phosphate aqueous solution is solvent, in brown volumetric flask, is settled to 2mL, as storing solution, otherThe reference substance solution of different quality concentration is obtained by storing solution dilution.
2. measure as claimed in claim 1 the method for Chlorogenic Acid of Flos Lonicerae and galuteolin content simultaneously,It is characterized in that, in ultrasonic wave extraction step, Honeysuckle Flower is crossed 65-80 mesh sieve in advance.
3. measure as claimed in claim 1 the method for Chlorogenic Acid of Flos Lonicerae and galuteolin content simultaneously,It is characterized in that, before quantitative analysis, carry out the preparation of need testing solution, comprising: extracting honeysuckle extractsLiquid is supplied weight with 70% ethanol water, shakes up, and filters, and crosses 0.22 μ m miillpore filter, obtains confessionTest sample solution.
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| CN104297374A (en) * | 2014-10-14 | 2015-01-21 | 南江县百草中药材有限公司 | Honeysuckle quality detection method |
| CN105486766A (en) * | 2015-10-13 | 2016-04-13 | 华南理工大学 | Method for determining content of three antioxidation active compositions in honeysuckle flower and plant thereof by employing HPLC |
| CN105911154A (en) * | 2016-02-01 | 2016-08-31 | 广西医科大学 | Method for determination of chlorogenic acid, galuteolin and total flavone content of honeysuckle |
| CN109633013A (en) * | 2018-12-29 | 2019-04-16 | 重庆医药高等专科学校 | A kind of honeysuckle multi objective quantitative analysis method |
| CN112444572A (en) * | 2019-08-30 | 2021-03-05 | 大连民族大学 | Method for measuring luteolin content in pteris crassipes by HPLC-DAD |
| CN112147265A (en) * | 2020-09-17 | 2020-12-29 | 天津市农业质量标准与检测技术研究所 | Honeysuckle anti-inflammatory quality marker screening and quality identification method and application |
| CN113552256B (en) * | 2021-07-20 | 2023-05-09 | 山东中医药大学 | Method for simultaneously measuring contents of 20 flavonoid components in honeysuckle |
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