CN103454229A - Method for discriminating proper picking time of chaenomeles speciosa nakai - Google Patents
Method for discriminating proper picking time of chaenomeles speciosa nakai Download PDFInfo
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Abstract
The invention discloses a method for discriminating the proper picking time of chaenomeles speciosa nakai. Firstly, the picked chaenomeles speciosa nakai is transversely cut up from the middle portion, then the color of a seed coat is observed, the color of the seed coat of the chaenomeles speciosa nakai under a natural lighting condition is yellow, according to the characteristic, the total organic acid of the active ingredients of the chaenomeles speciosa nakai is accumulated to reach a peak value of the fruit ripening and development process, and fruit density indicating the biological yield is also at a high level. Fruit water content related to the medicinal material yield is at a low level. The proper picking time of the chaenomeles speciosa nakai is judged according to the color of the seed coat, the method is simple and convenient, the proper picking time is easy to discriminate, and the method is supported by the detecting data of medicinal composition and the yield. The method is applied to picking of the medicinal chaenomeles speciosa nakai, contributes to regulating the picking time of the chaenomeles speciosa nakai and guaranteeing the quality and the yield of the chaenomeles speciosa nakai medicinal materials, and has good application value.
Description
Technical field
The present invention relates to Chinese crude drug planting technology field, relate in particular to a kind of pawpaw method of discrimination of suitable picking time of declaring.
Background technology
A surname pawpaw is the genunie medicinal materials of Chinese medicinal pawpaw (Chaenomeles Speciosa (Sweet) Nakai), within 2010, is listed in the national geography famous special product.As the saying goes: " spring adopts the oriental wormwood summer and becomes wormwood artemisia, has adopted autumn and has burnt when bavin " illustrates the importance of Chinese crude drug timely collecting.As the raw material of genunie medicinal materials, when a surname's pawpaw fruit should gather and be advisable, the elaboration that document is had nothing in common with each other.Have with ripening fruits and be used as medicine, also have with almost ripe fruit and be used as medicine, be one of problem of receiving much concern of pawpaw picking time always.
At present the method for discrimination of pawpaw picking time has following two kinds usually:
Method one: the color according to pericarp is determined the collecting period.2010 editions " Chinese pharmacopoeia (an one) regulation pawpaw is medicinal is almost ripe fruit, at summer, Qiu Erji, gathers, and with the fruit green-yellow, is advisable; Anhui Native standard (DB34/T283-2002) requires a surname pawpaw is medicinal to gather after Slight Heat, yellowish red color with pericarp and is advisable.
The place of production investigate to find, a surname pawpaw mainly contains 3 farm varieties, is respectively the arhat navel, apple is red and the sesame point, and different farm variety fruit colour features differ: the common green of arhat navel also has aubergine; Red many kermes of apple; The close living white point of sesame point pericarp, many greens.Be not that all a surname's pawpaw fruits pericarp when closely ripe can show green-yellow or yellowish red color, be difficult for grasping the nearly maturity state of a surname pawpaw according to fruit colour, so be difficult for grasping suitable picking time yet.
Method two: according to the plantation experience, determine the collecting period.A surname pawpaw is generally exhibition leaf florescence in mid-February to early March, and early April is the setting phase, and mid-April to late June is fruit expanding period, and July first arrival late July is fruit maturation early stage, after early August, is the fructescence.Place of production medicinal herb grower is mainly according to definite collecting periods such as pawpaw plantation experience, output, weather condition and busy situations.Control to picking time lacks standardization.
Estimate " flavor acid is good " and modern pharmacological research according to the pawpaw tradition, total organic acids is the effective constituent of pawpaw medicinal material; Oleanolic acid and ursolic acid are the " compositions of Chinese pharmacopoeia regulation pawpaw evaluation of medical materials' quality.The dynamic change of parameter in the ripe developmental process of a surname's pawpaw fruit that these " components groups " and fruit density and moisture etc. are relevant to root yield also has no report.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of pawpaw method of discrimination of suitable picking time of declaring.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of pawpaw method of discrimination of suitable picking time of declaring, fresh a surname pawpaw, from the cross section of middle part, is observed to kernel seed coat colour and presents yellow under the natural lighting condition, differentiate thus described a surname pawpaw in suitable picking time.
As preferably, also comprise following 4 auxiliary distinguishing rules; 4 auxiliary distinguishing rules meet for effective differentiation simultaneously:
(1) measure a surname's pawpaw fruit density, a surname's pawpaw fruit density of described suitable picking time is greater than 0.913g/cm
3;
(2) measure a surname's pawpaw fruit moisture, a surname's pawpaw fruit moisture of described suitable picking time is lower than 85.18%;
(3) measure a surname pawpaw total organic acids content, the water-soluble titratable total organic acids content of a surname pawpaw of described suitable picking time is higher than 11.16%;
(4) measure a surname's Oleanolic Acid in Chinese Flowering Quince ursolic acid total content, a surname's Oleanolic Acid in Chinese Flowering Quince ursolic acid total content of described suitable picking time is not less than 0.497%.
Through experiment, fresh a surname pawpaw of differing maturity, from the cross section of middle part, is observed to kernel seed coat colour under the natural lighting condition: a surname pawpaw kind skin has experienced the variation of white → yellow-white → yellow → tawny → brown.White is planted skin fruit in season crucial point in mezzanine level, and brown kind skin fruit in season crucial point is in the stage of ripeness, and yellow seed coat fruit in season crucial point is in the nearly stage of ripeness.Thus, when the observation kernel seed coat colour presents yellow under the natural lighting condition, differentiate described a surname pawpaw in suitable picking time.
The invention has the beneficial effects as follows:
Rule according to the ripe growth of a surname's pawpaw fruit and effective constituent cumulative change, consider two aspects of quality of medicinal material and output, the dynamic change of investigating index is associated with kernel seed coat colour, the differentiation of timely collecting is implemented in the color identification of kind of skin the most at last, gather very easy operability is provided for " preferentially in good time ", ensure a surname pawpaw medicinal material good quality and high output, quality controllable purpose to reach.
Embodiment
1 instrument and material
Instrument Agilent1100 high performance liquid chromatograph (comprises G1311A pump, G1322 degasser, G1313AZ automatic sampler, G1313A column oven, G1315DAD; The ChemStation chromatographic work station); BP221D electronic balance (Sartorius company); PHs-3CT type precision acidity meter (Shanghai great Pu Instrument Ltd.); KQ-250DB numerical control ultrasonic cleaner (Kunshan City, Jiangsu Province ultrasonic instrument company limited); Milli-Q laboratory ultrapure water system (Merck Millipore company); 101-B2A electric drying oven with forced convection (Shanghai Electric Power instrument plant)
Material a surname pawpaw gathers from the new Tian Town of Xuancheng Profile, anhui Province ，Jing Anhui, pawpaw planting base professor Peng Huasheng of university of TCM a surname and is accredited as chaenomeles lagenaria Chaenomeles sepciosa (Sweet) Nakai fruit; Fresh fruit is adopted rear 2 parts that are divided at random, and a part is as moisture and density measurement, and a part is put in boiling water and scalded to the crust canescence, and double vertical profile shines dry grinding standby composition measurement and use.Malic acid, oleanolic acid and ursolic acid reference substance are purchased from National Institute for Food and Drugs Control; Methyl alcohol is chromatographically pure; Potassium Hydrogen Phthalate is standard reagent; It is pure that other reagent are analysis; Water is ultrapure water.
2 methods and result
2.1 determine the time range that investigate applicable picking time
New Tian Town, Xuancheng City, Anhui Province is described as the township of a surname pawpaw.Local medicinal herb grower gathers in recent years and declares pawpaw many when Slight Heat, and while gathering, long span is approximately more than 20 days.By the examine on the spot of situation that a surname pawpaw is born fruit, the start time that will investigate picking time fixes on the Summer Solstice in 24 solar term, and during heat, a surname's pawpaw fruit shedding phenomenon is serious, therefore terminal fixes on the Limit of Heat nearby.The timing node of investigating is respectively in the Summer Solstice, Slight Heat, Great Heat, the beginning of autumn, the Limit of Heat (investigating duration from late June to late August, respectively in 2010 and 2011 continuous 2 years).
2.2 different a surname pawpaw kernel seed coat colours of gathering period
Observe a surname pawpaw fruit colour, find ripe after pericarp equal yellow and helvolus in various degree, but various, deep mixed at nearly maturity stage fruit colour, feature is difficult for holding; By the bright pawpaw of harvesting, from the middle part cross section, the immediate observation kernel seed coat colour is observed under natural light, the variation of kernel seed coat colour experience white → yellow-white → yellow → tawny → brown, and kernel seed coat colour is simple, and it is clear to change, as shown in table 1.
The different stage of ripeness kernel seed coat colours of table 1 a surname pawpaw fruit
| Observation period | The Summer Solstice | Slight Heat | Great Heat | The beginning of autumn | The Limit of Heat |
| Kernel seed coat colour | White | Yellow-white | Yellow | Tawny | Brown |
2.3 different a surname pawpaw moistures of gathering period
Determination of moisture is with reference to 2010 editions " Chinese pharmacopoeia (one one) appendix IX H first methods (oven drying method), be about to declare the pawpaw sample to thinly slice and be placed in the double dish that is dried to constant weight, put in drying box dry, extremely the double dried difference of weighing is no more than 5mg, weight according to less loss before and after dry, calculate the moisture of a surname pawpaw, the results are shown in Table 2.
Table 2 difference is declared pawpaw fresh fruit moisture (%) period of gathering
2.4 different a surname pawpaw density of gathering period
Density measurement adopts balance weighing and draining to survey volumetric method, gets at random 30 of fresh a surname pawpaws, weigh one by one, and measurement volumes, divided by volume, obtain the density of pawpaw fruit with pawpaw weight, the results are shown in Table 3.
Table 3 difference is declared pawpaw fresh fruit density (g/cm the period of gathering
3)
2.5 water-soluble titratable total organic acids content
Adopt potentiometric titration, according to document (Zhu Chenchen, Cheng Jingjing, Xie Xiaomei, etc. the water-soluble total organic acids content of Chinese medicinal pawpaw is relatively. R&D of modern TCM and practice, 2011,25 (3): 75) slightly make improvements.Specifically be determined as: get the about 1.5g of a surname's pawpaw fine powder, accurately weighed, precision adds water 50ml, weighed weight, ultrasonic processing (power 250W, frequency 40KHz) 30min, let cool, and water is supplied the weight of less loss, shake up, filter, precision measures subsequent filtrate 25mL, by potentiometric titration, with the NaOH standard solution titration of having demarcated, record the pH value of titrant consumption volume and titrate, adopt Origin6.0Professional Software on Drawing a surname pawpaw sample solution titration curve, by secondary difference quotient interpolation method, determine titration end-point; Be calculated as follows a surname's water-soluble titratable total organic acids content of pawpaw (in malic acid).
In formula: C is Concentration of Sodium Hydroxide Solution Standard (mol/L), consumes the volume (ml) of standard solution of sodium hydroxide when V is stoichiometric point, V
0consume the volume (ml) of standard solution of sodium hydroxide during for blank, the molal weight that M is malic acid (g/mol), W is a surname's pawpaw quality of medicinal material (g).Titration results is in Table 4.
Table 4 difference is declared the water-soluble titratable total organic acids content of pawpaw dry product (%) period of gathering
2.6 oleanolic acid and ursolic acid content
Adopt high performance liquid chromatography (1. Chinese Pharmacopoeia Commission. Pharmacopoeia of People's Republic of China. one one. Beijing: Chinese Medicine science and technology publishing house, 2010:57; 2. Lv Mei is red, and Xie Xiaomei looks into the filial piety post, etc. oleanolic acid and ursolic acid content in rp-hplc determination pawpaw Medicinal material and cut crude drug. Anhui Chinese Medicine College journal, 2010,29 (3): 72).
2.6.1 chromatographic condition
Chromatographic column: Shim-pack CLC-ODS (M) post (250mm * 4.6mm, 5 μ m); Mobile phase: methanol-water-glacial acetic acid-triethylamine (265:35:0.1:0.05); Flow velocity: 0.6mL/min; Detect wavelength: 210nm; Column temperature: 20 ℃; Sample size: 20 μ L.
2.6.2 the preparation of reference substance solution
Precision takes oleanolic acid reference substance 2.01mg, ursolic acid reference substance 2.06mg, puts respectively in the 5mL measuring bottle, adds methyl alcohol and dissolves and be diluted to scale, shakes up, and obtains oleanolic acid, ursolic acid reference substance stock solution.
2.6.3 sample solution preparation
Get the about 0.5g of a surname's pawpaw medicinal material fine powder, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25mL, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40KHz) 20min, let cool, weighed weight again, supply the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, 0.45 μ m membrane filtration, obtain.
2.6.4 sample determination
By under " 2.6.3 ", preparing need testing solution, by " 2.6.1 " lower chromatographic condition sample introduction, to analyze, external standard method is calculated respectively oleanolic acid and ursolic acid content, and calculates Different Harvesting Time a surname's Oleanolic Acid in Chinese Flowering Quince and ursolic acid content adds and is worth, and the results are shown in Table 5.
Table 5 difference is declared pawpaw dry product oleanolic acid (OA) and ursolic acid (UA) content (%) period of gathering
2.7 interpretation of result
As known from Table 1, in the investigation of 2 months by a definite date, a surname pawpaw kind skin has experienced the variation of white → yellow-white → yellow → tawny → brown.White is planted skin fruit in season crucial point in mezzanine level, and brown kind skin fruit in season crucial point, in the stage of ripeness, yellow fruit in season crucial point in the nearly stage of ripeness.
As known from Table 2, a surname pawpaw water cut is in relatively low level when the fruit prematurity, and along with Fruit development, water cut increases larger gradually, when fruit kind skin is brown, reaches highest level; Water cut is high, and the medicinal material rate of giving money as a gift is just low.Within continuous 2 years, follow the tracks of the result detected close.
As known from Table 3, a surname's pawpaw variable density presented in prematurity and maturity stage density lower than the nearly maturity stage, and while planting Beijing opera white, the density maximum, show decline situation subsequently; Density is large, and the biological yield of fruit is just high.Within continuous 2 years, follow the tracks of the result detected close.
As known from Table 4, in a surname's pawpaw fruit, water-soluble total organic acids content is fuctuation within a narrow range in prematurity to nearly maturation, reaches maximal value when kind of a skin is yellow, shows subsequently obvious downtrending; Between probation, the total organic acids content is obvious, and the variation range of average content (%) is 8.77～13.68; Within continuous 2 years, follow the tracks of the result detected close.
As known from Table 5, a surname pawpaw, investigating time period content of oleanolic acid fuctuation within a narrow range, slightly descends, and ursolic acid content slightly rises; Oleanolic acid and ursolic acid total amount (%) change not obvious, and mean value ± SD is 0.498 ± 0.015.This and existing result of study similar (Cheng Jingjing, etc. distribution and the dynamic change of ursolic acid oleanolic acid in the loguat leaf loquat flower for Zhang Shenglong, Xie Xiaomei. Chinese Pharmaceutical Journal, 2013,48 (6): 419).
In sum, so will select to declare pawpaw to gather within suitable picking time, because gather too early, the active component accumulation is not enough; Gathered evening, fruit water content increases, pulp pine bubble, medical material quanlity and production declining.
The physical and chemical index of declaring pawpaw suitable picking time and the kernel seed coat colour in the present embodiment, investigated have larger relevance, and change and the most obviously can distinguish with kernel seed coat colour, therefore, when the kernel seed coat colour of usining is yellow as a surname's distinguishing rule of pawpaw suitable picking time, the Quality and yield that can ensure a surname pawpaw medicinal material meets Chinese Pharmacopoeia regulation and physical and chemical index requirement, and very convenient operation is grasped again.
Above-described embodiment of the present invention, do not form limiting the scope of the present invention.Any modification of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in claim protection domain of the present invention.
Claims (2)
1. declare the pawpaw method of discrimination of suitable picking time for one kind, it is characterized in that: fresh a surname pawpaw, from the cross section of middle part, is observed to kernel seed coat colour and presents yellow under the natural lighting condition, differentiate thus described a surname pawpaw in suitable picking time.
2. method of discrimination according to claim 1, characterized by further comprising following 4 auxiliary distinguishing rules; 4 described auxiliary distinguishing rules meet for effective differentiation simultaneously:
(1) measure a surname's pawpaw fruit density, a surname's pawpaw fruit density of described suitable picking time is greater than 0.913g/cm
3;
(2) measure a surname's pawpaw fruit moisture, a surname's pawpaw fruit moisture of described suitable picking time is lower than 85.18%;
(3) measure a surname pawpaw total organic acids content, the water-soluble titratable total organic acids content of a surname pawpaw of described suitable picking time is higher than 11.16%;
(4) measure a surname's Oleanolic Acid in Chinese Flowering Quince ursolic acid total content, a surname's Oleanolic Acid in Chinese Flowering Quince ursolic acid total content of described suitable picking time is not less than 0.497%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301122A (en) * | 2015-04-06 | 2016-02-03 | 查孝柱 | Method for determination of contents of oleanolic acid and ursolic acid in kiwi fruit oil through high performance liquid chromatography |
| CN105875173A (en) * | 2016-06-14 | 2016-08-24 | 江苏茅山地道中药材种植有限公司 | Interplanting method of chaenomeles speciosa and rhizome areactylodis lanceae |
| CN106483220A (en) * | 2016-10-13 | 2017-03-08 | 山东省分析测试中心 | A kind of detection method of chaenomeles thibetica Yu active component and the construction method of multi objective quantitative finger print atlas |
| CN107184681A (en) * | 2017-06-05 | 2017-09-22 | 山东省中医药研究院 | A kind of Habitat producing concocting method of Xuancheng's pawpaw |
| CN108426960A (en) * | 2018-05-15 | 2018-08-21 | 吉林省白山本苜药业有限公司 | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301122A (en) * | 2015-04-06 | 2016-02-03 | 查孝柱 | Method for determination of contents of oleanolic acid and ursolic acid in kiwi fruit oil through high performance liquid chromatography |
| CN105875173A (en) * | 2016-06-14 | 2016-08-24 | 江苏茅山地道中药材种植有限公司 | Interplanting method of chaenomeles speciosa and rhizome areactylodis lanceae |
| CN105875173B (en) * | 2016-06-14 | 2020-07-10 | 江苏茅山地道中药材种植有限公司 | Interplanting method of chaenomeles speciosa and atractylis lancea |
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| CN106483220B (en) * | 2016-10-13 | 2018-10-02 | 山东省分析测试中心 | A kind of detection method of chaenomeles thibetica Yu active constituent and the construction method of multi objective quantitative finger print atlas |
| CN107184681A (en) * | 2017-06-05 | 2017-09-22 | 山东省中医药研究院 | A kind of Habitat producing concocting method of Xuancheng's pawpaw |
| CN108426960A (en) * | 2018-05-15 | 2018-08-21 | 吉林省白山本苜药业有限公司 | The content assaying method of oleanolic acid in Fructus Chaenomelis and ursolic acid |
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