CN103454229B - A kind of method of discrimination of Xuancheng's pawpaw suitable collection period - Google Patents
A kind of method of discrimination of Xuancheng's pawpaw suitable collection period Download PDFInfo
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Abstract
The invention discloses a kind of method of discrimination of Xuancheng's pawpaw suitable collection period, first by the Xuancheng's pawpaw won from middle part cross section, then kernel seed coat colour is observed, under natural lighting condition, the color of Xuancheng's pawpaw seed coat presents yellow, under this feature, Xuancheng's pawpaw active component total organic acids accumulates the peak level be in fruit maturation developmental process, and the fruit density of mark biological yield is also in high level; And the fruit water content relevant with root yield is in low-level.The present invention judges Xuancheng's pawpaw suitable collection period by kernel seed coat colour, and method is easy, be easy to differentiate, and obtains the support that effective component and output detect data.This method is applied to medicinal Xuancheng's pawpaw to pluck, contributes to the picking time of specification Xuancheng's pawpaw, ensure the Quality and yield of Xuancheng's pawpaw medicinal material, there is good using value.
Description
Technical field
The present invention relates to Chinese crude drug planting technology field, particularly relate to a kind of method of discrimination of Xuancheng's pawpaw suitable collection period.
Background technology
Xuancheng's pawpaw is the genunie medicinal materials of Chinese medicinal pawpaw (ChaenomelesSpeciosa (Sweet) Nakai), within 2010, is listed in national geography famous special product.As the saying goes: " spring adopts oriental wormwood summer one-tenth wormwood artemisia, has adopted autumn when bavin burns ", illustrates the importance of Chinese crude drug timely collecting.As the raw material of genunie medicinal materials, Xuancheng's pawpaw fruit should be advisable when gathering, the elaboration that document is had nothing in common with each other.Have and be used as medicine with ripening fruits, also have and be used as medicine with almost ripe fruit, picking time is one of problem of receiving much concern of pawpaw always.
The method of discrimination of current pawpaw picking time has following two kinds usually:
Method one: determine the collecting period according to the color of pericarp.2010 editions " Chinese Pharmacopoeia " (one) regulation pawpaw is medicinal is almost ripe fruit, gathers, be advisable with fruit green-yellow at summer, Qiu Erji; Anhui Native standard (DB34/T283-2002) requires that Xuancheng's pawpaw is medicinal and gathers after Slight Heat, yellowish red color be advisable with pericarp.
The place of production is investigated and is found, Xuancheng's pawpaw mainly contains 3 farm varieties, and be respectively the red and sesame point of arhat navel, apple, different farm variety fruit colour feature differs: the common green of arhat navel, also has aubergine; Red many kermes of apple; The close raw white point of sesame point pericarp, many greens.And not all Xuancheng's pawpaw fruit pericarp when nearly maturation can show green-yellow or yellowish red color, not easily grasps the nearly maturity state of Xuancheng's pawpaw, therefore also not easily grasp suitable collection period according to fruit colour.
Method two: determine the collecting period according to plantation experience.Xuancheng's 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 first arrival late July in July is fruit maturation early stage, is the fructescence after early August.Place of production medicinal herb grower mainly determines the collecting period according to pawpaw plantation experience, output, weather condition and busy situation etc.Standardization is lacked to the control of picking time.
Evaluate " taste acid is good " and modern pharmacological research according to pawpaw tradition, total organic acids is the effective constituent of pawpaw medicinal material; Oleanolic acid and ursolic acid are the compositions that " Chinese Pharmacopoeia " specifies pawpaw evaluation of medical materials' quality.These " components groups " and fruit density also have no report with parameter dynamic changes in Xuancheng's pawpaw fruit maturation developmental process relevant to root yield such as moisture.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of discrimination of Xuancheng's pawpaw suitable collection period.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of discrimination of Xuancheng's pawpaw suitable collection period, by fresh Xuancheng's pawpaw after the cross section of middle part, under natural lighting condition, observe kernel seed coat colour present yellow, differentiate that described Xuancheng's pawpaw is in suitable collection period thus;
Also comprise following 4 subsidiary discriminant foundations, and 4 subsidiary discriminant are according to meeting for effective differentiation simultaneously:
(1) measure Xuancheng's pawpaw fruit density, the Xuancheng's pawpaw fruit density of described suitable collection period is greater than 0.913g/cm
3;
(2) measure Xuancheng's pawpaw fruit water content, the Xuancheng's pawpaw fruit water content of described suitable collection period is lower than 85.18%;
(3) measure Xuancheng's pawpaw total organic acids content, the water-soluble titratable total organic acids content of Xuancheng's pawpaw of described suitable collection period is higher than 11.16%;
(4) measure Xuancheng's pawpaw oleanolic acid and ursolic acid total content, Xuancheng's pawpaw oleanolic acid and the ursolic acid total content of described suitable collection period are not less than 0.497%.
Through experiment, by the fresh Xuancheng's pawpaw of differing maturity after the cross section of middle part, under natural lighting condition, observe kernel seed coat colour: Xuancheng's pawpaw seed coat experienced by the change of white → yellow-white → yellow → tawny → brown.White seed coat fruit in season crucial point is in mezzanine level, and brown seed coat color 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, under natural lighting condition, observe kernel seed coat colour when presenting yellow, differentiate that described Xuancheng's pawpaw is in suitable collection period.
The invention has the beneficial effects as follows:
Grow and the rule of effective constituent cumulative change according to Xuancheng's pawpaw fruit maturation, namely quality of medicinal material and output two aspects are considered, the dynamic change of inspection target is associated with kernel seed coat colour, the differentiation of timely collecting is implemented on the colour recognition of seed coat the most at last, gather for " preferentially in good time " and provide very easy operability, Xuancheng's pawpaw medicinal material good quality and high output is ensured, quality controllable object 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; 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 (MerckMillipore company); 101-B2A electric drying oven with forced convection (Shanghai Electric Power instrument plant)
Material Xuancheng's pawpaw gathers from Xuancheng's pawpaw planting base, Xuancheng Profile, anhui Province new Tian Town, is accredited as chaenomeles lagenaria Chaenomelessepciosa (Sweet) Nakai fruit through Anhui University of Chinese Medecine professor Peng Huasheng; Fresh fruit is adopted and is divided into 2 parts at random afterwards, and a part is used as moisture and density measurement, and a part is put in boiling water and scalded to crust canescence, double vertical profile, shines dry grinding standby composition measurement and uses.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 to be suitable for the time range investigated picking time
New Tian Town, Xuancheng City of Anhui Province is described as the township of Xuancheng's pawpaw.Local medicinal herb grower Xuancheng's pawpaw of gathering in recent years is many when Slight Heat, about more than 20 days of long span when gathering.By the examine on the spot of situation of bearing fruit to Xuancheng's pawpaw, the start time that picking time is investigated is fixed on the Summer Solstice in 24 solar term, nearby during heat, Xuancheng's pawpaw fruit shedding phenomenon is serious, therefore terminal fixes on the Limit of Heat.The timing node investigated 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).
The Xuancheng's pawpaw kernel seed coat colour of 2.2 different harvest time
Observe Xuancheng's 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 not easily held; By the fresh pawpaw of harvesting from middle part cross section, immediate observation kernel seed coat colour, observes under natural light, and the change of kernel seed coat colour experience white → yellow-white → yellow → tawny → brown, 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 colour of table 1 Xuancheng's 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 |
The Xuancheng's pawpaw moisture of 2.3 different harvest time
Determination of moisture is with reference to 2010 editions " Chinese Pharmacopoeia " (one) annex IXH first method (oven drying method), the double dish being placed in and being dried to constant weight is thinly sliced by Xuancheng's pawpaw sample, put in drying box dry, 5mg is no more than to double dried difference of weighing, according to the weight of dry front and back less loss, calculate the moisture of Xuancheng's pawpaw, the results are shown in Table 2.
Table 2 different harvest time Xuancheng's pawpaw fresh fruit moisture (%)
The Xuancheng's pawpaw density of 2.4 different harvest time
Density measurement is adopted and is weighed with scale and draining survey volumetric method, gets fresh Xuancheng's pawpaw 30 at random, weighs one by one, and measurement volumes, with pawpaw weight divided by volume, obtain the density of pawpaw fruit, the results are shown in Table 3.
Table 3 different harvest time Xuancheng's pawpaw fresh fruit density (g/cm
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 comparision contents of Chinese medicinal pawpaw. R&D of modern TCM and practice, 2011,25 (3): 75) slightly make improvements.Specifically be determined as: get Xuancheng's pawpaw fine powder and be about 1.5g, accurately weighed, precision adds water 50ml, weighed weight, ultrasonic process (power 250W, frequency 40KH
z) 30min, let cool, supply the weight of less loss with water, shake up, filter, precision measures subsequent filtrate 25mL, by potentiometric titration, with the NaOH standard solution titration of having demarcated, the pH value of record titrant consumption volume and titrate, adopt Origin6.0Professional Software on Drawing Xuancheng's pawpaw sample solution titration curve, by second derivative interpolation method determination titration end-point; Be calculated as follows the water-soluble titratable total organic acids content (in malic acid) of Xuancheng's pawpaw.
In formula: C is Concentration of Sodium Hydroxide Solution Standard (mol/L), consume the volume (ml) of standard solution of sodium hydroxide when V is stoichiometric point, V
0for consuming the volume (ml) of standard solution of sodium hydroxide during blank, M is the molal weight (g/mol) of malic acid, and W is Xuancheng's pawpaw quality of medicinal material (g).Titration results is in table 4.
The water-soluble titratable total organic acids content (%) of table 4 different harvest time Xuancheng's pawpaw dry product
2.6 oleanolic acids and ursolic acid content
Employing high performance liquid chromatography (1. Chinese Pharmacopoeia Commission. Pharmacopoeia of People's Republic of China. one. Beijing: China Medical Science Press, 2010:57; 2. Lv Mei is red, Xie Xiaomei, looks into 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-packCLC-ODS (M) post (250mm × 4.6mm, 5 μm); Mobile phase: methanol-water-glacial acetic acid-triethylamine (265: 35: 0.1: 0.05); Flow velocity: 0.6mL/min; Determined wavelength: 210nm; Column temperature: 20 DEG C; 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 5mL measuring bottle, adds methyl alcohol and dissolves and be diluted to scale, shake up, and obtains oleanolic acid, ursolic acid reference substance stock solution.
2.6.3 sample solution preparation
Get Xuancheng's pawpaw fine medicinal material powder and be about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25mL, close plug, weighed weight, ultrasonic process (power 250W, frequency 40KH
z) 20min, let cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, get subsequent filtrate, 0.45 μm of membrane filtration, to obtain final product.
2.6.4 sample determination
By preparing need testing solution under " 2.6.3 " item, analyze by chromatographic condition sample introduction under " 2.6.1 " item, external standard method calculates oleanolic acid and ursolic acid content respectively, and calculates Different Harvesting Time Xuancheng's pawpaw oleanolic acid and ursolic acid content adds and is worth, and the results are shown in Table 5.
Table 5 different harvest time Xuancheng's pawpaw dry product oleanolic acid (OA) and ursolic acid (UA) content (%)
2.7 interpretation of result
As known from Table 1, in the investigation of 2 months by a definite date, Xuancheng's pawpaw seed coat experienced by the change of white → yellow-white → yellow → tawny → brown.White seed coat fruit in season crucial point is in mezzanine level, and brown seed coat color 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, Xuancheng's pawpaw water cut is in relatively low level when fruit prematurity, and along with Fruit development, water cut increases comparatively large gradually, when fruit seed coat is brown, reaches highest level; Water cut is high, and medicinal material Drying rate is just low.The result of continuous 2 years tracing detection is close.
As known from Table 3, Xuancheng's pawpaw variable density presents in prematurity and maturity stage density lower than the nearly maturity stage, and during seed coat yellow-white, density is maximum, shows decline situation subsequently; Density is large, and the biological yield of fruit is just high.The result of continuous 2 years tracing detection is close.
As known from Table 4, in Xuancheng's pawpaw fruit, water-soluble total organic acids content is in prematurity near ripe in fuctuation within a narrow range, reaches maximal value, show obvious downtrending subsequently at seed coat in time yellow; Between probation, total organic acids content is obvious, and the variation range of average content (%) is 8.77 ~ 13.68; The result of continuous 2 years tracing detection is close.
As known from Table 5, Xuancheng's pawpaw is in investigation time period content of oleanolic acid fuctuation within a narrow range, and slightly decline, 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 (Zhang Shenglong, Xie Xiaomei, Cheng Jingjing, etc. the distribution in loguat leaf loquat flower of. ursolic acid oleanolic acid and dynamic change. Chinese Pharmaceutical Journal, 2013,48 (6): 419).
In sum, so Xuancheng's pawpaw will be selected to gather in suitable collection period, because gather too early, active component accumulation is not enough; Gathered evening, fruit water content increases, pulp pine bubble, medical material quanlity and production declining.
Physical and chemical index and the kernel seed coat colour of the suitable collection period Xuancheng's pawpaw investigated in the present embodiment have larger relevance, and the most obviously can distinguish with kernel seed coat colour change, therefore, using kernel seed coat colour in the distinguishing rule as Xuancheng's pawpaw suitable collection period time yellow, can ensure that the Quality and yield of Xuancheng's pawpaw medicinal material meets Chinese Pharmacopoeia regulation and physical and chemical index requirement, very convenient operation is grasped again.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (1)
1. a method of discrimination for Xuancheng's pawpaw suitable collection period, is characterized in that: by fresh Xuancheng's pawpaw after the cross section of middle part, observe kernel seed coat colour and present yellow under natural lighting condition, differentiates that described Xuancheng's pawpaw is in suitable collection period thus;
Also comprise following 4 subsidiary discriminant foundations, and 4 described subsidiary discriminant are according to meeting for effective differentiation simultaneously:
(1) measure Xuancheng's pawpaw fruit density, the Xuancheng's pawpaw fruit density of described suitable collection period is greater than 0.913g/cm
3;
(2) measure Xuancheng's pawpaw fruit water content, the Xuancheng's pawpaw fruit water content of described suitable collection period is lower than 85.18%;
(3) measure Xuancheng's pawpaw total organic acids content, the water-soluble titratable total organic acids content of Xuancheng's pawpaw of described suitable collection period is higher than 11.16%;
(4) measure Xuancheng's pawpaw oleanolic acid and ursolic acid total content, Xuancheng's pawpaw oleanolic acid and the ursolic acid total content of described suitable collection period are not less than 0.497%.
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| 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 |
| 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 |
| 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 |
| CN107184681B (en) * | 2017-06-05 | 2020-07-21 | 山东省中医药研究院 | Production place processing method of chaenomeles speciosa |
| 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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| KR101038935B1 (en) * | 2008-08-01 | 2011-06-07 | 대한민국 | Method and color chart for estimating ripening degree of fuji apples |
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