CN102397384B - Heartleaf houttuynia herb eye drops and preparation method thereof - Google Patents

Heartleaf houttuynia herb eye drops and preparation method thereof Download PDF

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CN102397384B
CN102397384B CN2011103612580A CN201110361258A CN102397384B CN 102397384 B CN102397384 B CN 102397384B CN 2011103612580 A CN2011103612580 A CN 2011103612580A CN 201110361258 A CN201110361258 A CN 201110361258A CN 102397384 B CN102397384 B CN 102397384B
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dissolve
distilled liquid
herba houttuyniae
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CN102397384A (en
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吴飞驰
钟军
仇萍
熊兴耀
向卫国
曾维军
李苏翠
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ZHENGQING PHARMACEUTICAL GROUP CORP Ltd HUNAN PROV
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ZHENGQING PHARMACEUTICAL GROUP CORP Ltd HUNAN PROV
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Abstract

The invention discloses heartleaf houttuynia herb eye drops and a preparation method thereof. On the basis of the conventional production process, tent-planted heartleaf houttuynia herb consisting of an aboveground part and an underground part in a specific ratio is taken as a raw material, so that the quality of products of different batches is stable and uniform; and the dosage of polysorbate 80 is reduced, the cell membrane cracking action, irritation, haemolysis and histamine release (sensitization) caused by the polysorbate 80 are lowered, and the administration safety is improved.

Description

A kind of cordate houttuynia eye drops and preparation method thereof
Technical field
The present invention relates to a kind of eye drop and preparation method thereof, particularly eye drop of making of a kind of Herba Houttuyniae and preparation method thereof.
Background technology
Herba Houttuyniae is the whole herb with root of Saururaceae herbaceos perennial Herba Houttuyniae Houttuynia cordata Thunb., have another name called Herba Houttuyniae, purple Ji, hog snout hole, Rhizoma Rohdeae Japonicae etc., pungent stench flavor is arranged after its Fresh Plants fragmentation, being distributed widely in Central China, the southeast and ,You Yi Hunan, each provinces and regions, southwest, Hubei, Sichuan, Jiangsu etc. economizes in the majority.Herba Houttuyniae has the effect of heat-clearing and toxic substances removing, eliminating carbuncle evacuation of pus, inducing diuresis for treating stranguria syndrome, clinical for lung abscess vomiting pus, expectorant dyspnea of heat type cough, the disease such as hematodiarrhoea, pyretic stranguria, carbuncle sore tumefacting virus.Research shows, in Herba Houttuyniae, contains the compositions such as volatile ingredient, flavonoid, organic acid, sterols, alkaloids.Cordate houttuynia eye drops is to obtain through the steam distillation preparation, and main component is its volatile ingredient.It is edible that Herba Houttuyniae mainly is made for vegetable with young stem and leaf and subterraneous stem, but Herb using fresh herb or dry be used as medicine, by health ministry, formally be defined as one of the resource of the great exploitation potential for its of " being medicine, is again food ", day by day receive people's concern.Herba Houttuyniae is always wild plant, since the beginning of the forties in last century, carries out artificial culture, but, due to winter low temperature, can not guarantee the growth of Herba Houttuyniae aerial parts, therefore the supply of Herba Houttuyniae is got into a difficult position.
Summary of the invention
The invention discloses a kind of cordate houttuynia eye drops and preparation method thereof.
The present invention seeks to be achieved by the following scheme:
The preparation method of cordate houttuynia eye drops of the present invention comprises the steps:
(1) according to mass ratio, be 1: 1-3.5 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 1000-3000 parts by volume, then carry out redistillation, collect re-distilled liquid 700-1300 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰-3 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 2, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 10 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention also preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 3, carry out vapor distillation, collect just distillate 1500 parts by volume, then carry out redistillation, collect re-distilled liquid 850 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.9 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 8 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention also preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 1.5, carry out vapor distillation, collect just distillate 2500 parts by volume, then carry out redistillation, collect re-distilled liquid 1300 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.6 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 15 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 2, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.7 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 2, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.9 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 2, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 3 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 1.5, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
The preparation method of cordate houttuynia eye drops of the present invention preferably includes following steps:
(1) according to mass ratio, be to get fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions at 1: 2.5, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) re-distilled liquid after step (2) is processed, used the filter element of 0.45 μ m and 0.22 μ m to filter, embedding, 115 ℃ sterilizing 32 minutes, obtain cordate houttuynia eye drops.
Wherein, between above-mentioned weight portion and parts by volume, be the relation of g/ml.
Herba Houttuyniae of the present invention refers to the Herba Houttuyniae of greenhouse gardening, and the greenhouse gardening method comprises the steps:
(1) booth construction: comprise the bow type of cross direction profiles or class bow type crossbeam, the horizontal bar or the cross bar that vertically distribute; Adopt long 25-30m, wide 5-6m, the transparent PVP thin film of high 3-3.5m; Girder: bamboo; Framework: steel pipe; Garden put up a shed on the ground frame, lid thin film, form the warmhouse booth main body;
(2) plantation
1. ground, garden is prepared: select pH5.0~6.5, content of organic matter 20-25g/kg, full nitrogen is 1.0-1.5g/kg, and quick-acting potassium content is 100-150mg/kg, and available phosphorus contents is the sandy loam of 40-50mg/kg;
2. wholely: the ground, garden that will select, after before sowing, being turned in ground, divide ,Ji railway carriage or compartment, railway carriage or compartment wide 5-6m by following distance, railway carriage or compartment furrow width 1-2m, dark 0.4-0.5m, smash to pieces railway carriage or compartment face earth smooth after loose fertilise;
3. sowing: select the unblemished fish raw meat grass seeds stem with 1-2 eye, disseminate in garden on the ground by the application rate of 40-50kg/ mu; Then earthing, thickness of earth-fill cover is advisable with 10-15cm; All can sow the whole year;
4. overlay film time: directly put up plastic sheeting or postpone and putting up again in several days after sowing finishes;
(3) management
1. thermoregulation is controlled: budding time (till namely sending out 1-2 bud to each kind stem after the plantation),, in ground, garden plantation layer, daytime temperature is controlled at 20-25 ℃ of scope; After this cool the temperature to 20 ℃;
2. irrigate: will keep soil moisture to be greater than 75% to whole trophophase garden, water 3-5 time;
3. topdress: in neat seedling stage, carry Seedling, every mu of 1000-1500kg with the farm manure become thoroughly decomposed, during fertilising, every mu separately adds carbamide 15-20kg, nitrogen, phosphorus, K composite fertilizer 5-8kg, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16: 15 or 16: 15 or 16, dissolve in wherein and apply in the lump; Stem, leaf vigorous period (mid-May-to mid-June), every mu of farm manure 1000-1500kg that executes to become thoroughly decomposed, during fertilising, every mu separately adds carbamide 10-12kg and dissolves in wherein and apply in the lump;
4. weeding: weeds, with seeing with removing, avoid striving rich water with Seedling.
Ground, garden is prepared preferably: content of organic matter 20-25g/kg, and full nitrogen is 1.0-1.5g/kg, and quick-acting potassium content is 100-150mg/kg, and available phosphorus contents is 40-50mg/kg;
Before ground, described garden is prepared to refer to sowing, execute well-rotted farmyard manure barnyard manure, compost or make compost 1000-1500kg and nitrogen, phosphorus, K composite fertilizer 100-150kg for every mu, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16: 15 or 16: 15 or 16; Content of beary metal soil high, that pollution is heavy is not suitable for choosing and does ground, garden;
The described overlay film time must carry out before temperature is reduced to 15 ℃.
Method of planting herba houttuyniae in greenhouse of the present invention especially can solve winter, the under-supply problem of fresh fish raw meat grass aerial parts in spring (November-May), make the Herba Houttuyniae aerial parts also can normal growth in winter, spring, and the greenhouse gardening Herba Houttuyniae has also shortened its period of duration, its output is significantly higher than bare area plantation.
Eye drop of the present invention is on existing production technology basis, and selecting the Herba Houttuyniae of the greenhouse gardening of Herba Houttuyniae aerial parts and under ground portion special ratios is raw material, has guaranteed the steady quality homogeneous of the different batches product of product of the present invention; The present invention has also reduced the polyoxyethylene sorbitan monoleate consumption, has reduced effect and the zest caused, hemolytic and the histamine release (sensitization) of the ruptured cell film that polyoxyethylene sorbitan monoleate causes, has improved drug safety.
Following experimental example and embodiment are for further illustrating but being not limited to the present invention.
Experimental example one: greenhouse gardening mode (seeing embodiment mono-) and the bare area planting patterns experiment that compares
1, with the greenhouse gardening mode of winter planting and bare area planting patterns, compare in ambient temperature and humidity and Herba Houttuyniae growth result.The results are shown in Table one.
Table one: the comparison of greenhouse gardening mode temperature, humidity and growth result
Figure BDA0000108687760000061
Upper table explanation: 1. the temperature of greenhouse gardening is more constant.2. greenhouse gardening Herba Houttuyniae growth is fast, compares than the Herba Houttuyniae of the bare area of same period plantation, and plant strain growth is the fast growth of aerial parts plant height especially soon; Simultaneously, the growth of single-strain fresh weight is also higher.
2, the comparison of booth and bare area plantation Herba Houttuyniae period of duration
The greenhouse gardening Herba Houttuyniae, to different growing stages such as seeding stage (1.3), neat seedling stage (1.20), the envelope departure date (2.28) and florescence (5.13), the required time is respectively 2 weeks, 4 weeks, February and May from epiphragma day (12.21).And bare area plantation Herba Houttuyniae is respectively February, March, 3.5 months and May (table two) to seeding stage (2.20), neat seedling stage (3.17), the envelope departure date (4.2) and (5.13) required time in florescence from December 21 days.
Table two: the comparison of booth and bare area plantation Herba Houttuyniae period of duration
Figure BDA0000108687760000062
Above data declaration: owing to having used the greenhouse gardening Herba Houttuyniae, especially in the 12-3 month, significantly improved the environmental conditions such as temperature and humidity of its growth, so the Herba Houttuyniae fast growth of greenhouse gardening at the growth period of Herba Houttuyniae; With the Herba Houttuyniae of bare area plantation, compare, shortened greatly that it is emerged, time and the natural law of Qi Miao and envelope row.
3, the comparison of booth and the bare area plantation Herba Houttuyniae speed of growth
Booth and the bare area plantation Herba Houttuyniae speed of growth the results are shown in Table three.
Table three: the comparison of booth and bare area plantation Herba Houttuyniae aerial growth speed
Upper table explanation: the early growth temperature (winter) that has guaranteed Herba Houttuyniae due to greenhouse gardening, so the aerial parts of Herba Houttuyniae has reached respectively 0.39cm/d and 0.76cm/d in the day growth speed in February and March, that bare area is planted is 0.003cm/d and 0.05cm/d; Due to the epiphragma of having taken off booth April, the temperature inside and outside booth is identical, makes the day growth velocity ratio of both aerial partss more approaching; And, because temperature now is the temperature of Herba Houttuyniae optimum growh, cause the speed of growth of now bare area plantation also large; In May, both day growth speed has reduced again, but the day growth speed of greenhouse gardening Herba Houttuyniae aerial parts is at 0.70cm/d, the bare area plantation be the Herba Houttuyniae of 0.21cm/d. greenhouse gardening, emerge morning and fast growth per month of aerial parts not only; From the actual production of collection period (May), compare, every mu up to 3600kg.And the Herba Houttuyniae of bare area plantation, April aerial parts day growth just than faster, but be reduced to again 0.21cm/d May, every mu of the actual production of collection period (May) also only has 2400kg.
4, the comparison of booth and bare area plantation Herba Houttuyniae volatile oil main chemical compositions content
Detect the content of the volatile oil main chemical compositions of Herba Houttuyniae, the results are shown in Table four.
Table four: the assay result of booth and bare area plantation Herba Houttuyniae main chemical compositions
Figure BDA0000108687760000071
A:4-methyl isophthalic acid-isopropyl-3-cyclohexene-1-alcohol
B:2-(4-methyl-3-cyclohexenyl group) isopropyl alcohol
C: borneol acetate
D: methylnonanone
The explanation of upper table: 1 with the comparing of bare area plantation, the aerial parts of greenhouse gardening was emerged early 2 months, just its volatile oil content can be detected in February; And the bare area plantation, now also do not grow aerial parts.2, the content of the Herba Houttuyniae of the content of the volatile oil main chemical compositions of greenhouse gardening and the bare area plantation same period is close.
The screening experiment of different technologies parameter in experimental example two, planting herba houttuyniae in greenhouse situation
1, the different cropping patterns of greenhouse gardening Herba Houttuyniae relatively
At seeding time, three kinds of cropping patterns have been adopted in booth experiment: 1. booth; 2. booth+mulch film (seeing embodiment mono-); 3. booth+mulch film+lamp, after Qi Miao (January 20), throw off mulch film, and the comparative result of three kinds of cropping pattern Herba Houttuyniae speed of emergence is in Table five.
Table five: the comparison of booth Different Ways of Planting Herba Houttuyniae speed of emergence
Figure BDA0000108687760000081
Annotate: the letter representative is 5% level of difference statistically.
From the speed of emergence of the greenhouse gardening pattern of upper table, can illustrate: the third (booth+mulch film+lamp) slightly is better than the second (booth+mulch film), but both between no significant difference; The first (booth) is obviously poor.But because the input of the third cropping pattern (booth+mulch film+lamp) in lamp and the electricity charge obviously increases to some extent than the second cropping pattern (booth+mulch film), therefore, from speed of emergence and economic two aspects of Herba Houttuyniae, consider, this experiment selected " booth+mulch film " is as the cropping pattern of booth.
2, the different sowing times of greenhouse gardening Herba Houttuyniae
Experiment is sowed a collection of per month, sows altogether 12 batches, and Mei Pimei community sown area is 10m 2, 3 repetitions.In the flowers and fruits later stage, gather, while gathering, minute cell measurement above and below ground part weight and volatile oil content and methylnonanone content.Ethereal oil and methylnonanone extraction and determination are undertaken by Chinese Pharmacopoeia (2010 editions), speed of emergence, output and the volatile oil content of its different sowing times the results are shown in Table six.
Table six greenhouse gardening Herba Houttuyniae Different Sowing Dates speed of emergence, output and volatile oil content are relatively
Result shows: (1) Herba Houttuyniae all can be cultivated throughout the year; (2) Herba Houttuyniae of sowing all can also can reach the basic demand of gathering in the regular period by germination and growth per month.But the Herba Houttuyniae of sowing respectively has characteristics per month, as the Herba Houttuyniae sowed the 1-2 month can be when gathering output not high, although Herba Houttuyniae output when gathering of sowing the 3-5 month is higher, ethereal oil content is also higher; The Herba Houttuyniae of sowing the 6-8 month may affect sprouting because temperature was too high at that time, therefore sprout time will be grown than the time of spring or early summer (the 2-5 month) sowing, while gathering, output is not high yet; The Herba Houttuyniae of sowing the 9-12 month can obtain more stable output and higher ethereal oil content, also not very long to the appropriation of land time.
3, the difference of greenhouse gardening Herba Houttuyniae sowing sowing quantity
Testing random Quarter Design ,Mei community sown area is 10m 2, 3 repetitions, mainly compared on the ground and under ground portion yield per unit area and ethereal oil content, the results are shown in Table seven.
Table seven greenhouse gardening Herba Houttuyniae different seeding quantity compares the impact of output and volatile oil content
Figure BDA0000108687760000091
Presentation of results, the Herba Houttuyniae application rate has certain influence to output, and the output that application rate is large is higher.The output of application rate 10kg/ mu is obviously on the low side, and application rate is not a lot of for amount for the output of 40-60kg/ mu differs; And ethereal oil content is subjected to the impact of application rate not fairly obvious.Therefore, experiment determines that the sowing quantity of greenhouse gardening Herba Houttuyniae is 40-50kg/ mu.
4, the fertilizer amount of greenhouse gardening Herba Houttuyniae
Carbamide (X is established in experiment 1), calcium superphosphate (X 2), potassium sulfate (X 3) and pig manure (X 4) 4 factors, each factor is established 5 levels.By the secondary universal rotary combination design of orthogonal test, obtain the processing of 20 Different proportion of fertilizers, each is processed and repeats 3 times.Then according to the yield result of each processing, principle and the method for application universal rotational regression modular design are carried out regression analysis, and the mathematical model of trying to achieve between output and each factor is Y=114.05+3.52X 1+ 3.28X 2+ 5.28X 3+ 8.29X 4-1.49X 1X 2-1.11X 1X 3-0.17X 1X 4-0.17X 2X 3-1.11X 2X 4+ 1.48X 3X 4.If according to this formula, calculate by per mu yield Herba Houttuyniae 3600kg, need carbamide 150kg, calcium superphosphate 325kg, potassium sulfate 110kg, pig manure 470kg.
The fertilising of Herba Houttuyniae in general fertilizer with quick-acting fertilizer, to be combined effect better, fertilizer mainly is used as base manure, topdresses and with thin night soil, is used in conjunction with instant nitrogenousfertilizer, foliage dressing is mainly potash fertilizer.Therefore, determine that the dose in base and method are: 1. base manure.Execute well-rotted farmyard manure (barnyard manure, compost or make compost) 1000-1500kg for every mu, nitrogen, phosphorus, K composite fertilizer (15 or 16: 15 or 16: 15 or 16) 100-150kg.2. topdress.Early execute and gently execute seed manure, Qi Miaoshi, the farm manure become thoroughly decomposed of use is carried Seedling, every mu of 1000-1500kg, during fertilising, every mu separately adds carbamide 15-20kg, and nitrogen, phosphorus, K composite fertilizer (15 or 16: 15 or 16: 15 or 16) 5-8kg dissolves in wherein and applies in the lump.When stem, leaf vigorous growth (mid-May-to mid-June), every mu of farm manure 1000-1500kg that executes to become thoroughly decomposed, during fertilising, every mu separately adds carbamide 10-12kg and dissolves in wherein and apply in the lump.
5, the water consumption of greenhouse gardening Herba Houttuyniae
Due to Herba Houttuyniae dark and damp characteristic in the family way, therefore in the Herba Houttuyniae cultivation, keep field moisture and irrigation conditions very important.The impact research of different moistures on the output of the germination percentage of Herba Houttuyniae germination period and the envelope departure date (Qi Miao-beginning flower) and flowering fruit bearing stage has been carried out in test, the results are shown in Table eight.
The impact of table eight soil moisture on the Herba Houttuyniae growth
Figure BDA0000108687760000101
Above result shows: (1) will guarantee that the germination percentage of Herba Houttuyniae must keep soil moisture content in 90% left and right; (2) soil moisture is fairly obvious to the yield effect from the envelope departure date and flowering fruit bearing stage Herba Houttuyniae.Envelope departure date moisture preferably is controlled at 90% left and right, and the soil water content of flowering fruit bearing stage can not be lower than 80%.
6, the greenhouse gardening Herba Houttuyniae gathers
Experimental comparative analysis the best collecting time of greenhouse gardening Herba Houttuyniae on the impact of its biological yield and volatile oil content, result of study is in Table nine.
The impact of table nine different harvest time Herba Houttuyniae output and ethereal oil content
Figure BDA0000108687760000102
The gather May output of Herba Houttuyniae aerial parts of the presentation of results of table nine has just reached the output requirement substantially, aerial parts output reached maximum and can remain to JIUYUE always July-August, but after October, because temperature starts continuous decline, aerial parts starts the fallen leaves of progressively withering, and output progressively descends; Under ground portion output, just starting to have very fast growth the 7-8 month, reaches high value to mid-October, tend towards stability to November.Aerial parts ethereal oil content reaches high in May, and the 6-7 month is more stable, and descend August to some extent, the fastest to the JIUYUE decrease speed; Under ground portion rises on the way, just descends to October.
From the output of Herba Houttuyniae Different Harvesting Time and the variation of volatile oil content, prosperous long-term end and lag phase (the 5-9 month) are the best collecting times of aerial parts, if need of production late April also can gather; And the best collecting time of under ground portion is generally the 7-9 month, but also can be deferred to October.Producing Herba Houttuyniae used is herb, comprehensive aerial parts and under ground portion, and experiment determines that the 5-10 month is the best collecting time of Herba Houttuyniae.
Conclusion:
Above result demonstration, greenhouse gardening is compared with the Herba Houttuyniae of bare area plantation, has improved the environment such as temperature and humidity of Herba Houttuyniae growth, therefore:
1, greatly shortened the growth time of Herba Houttuyniae, especially from the seeding stage to sealing the departure date;
2, the Herba Houttuyniae of greenhouse gardening has guaranteed can grow aerial parts in the winter time, and the day growth velocity ratio of aerial parts is larger; Its output is significantly higher than the bare area plantation;
3, the content of the Herba Houttuyniae of the content of the volatile oil main chemical compositions of the Herba Houttuyniae of greenhouse gardening and the bare area plantation same period is close.Has same medical value.
4, use the greenhouse gardening Herba Houttuyniae, can improve significantly winter and can not receive the problem of the bright Herba Houttuyniae that meets the pharmacopeia requirement because temperature is low.
The screening of experimental example three Herba Houttuyniae medicinal part ratios
The raw material of cordate houttuynia eye drops of the present invention is bright Herba Houttuyniae, and medicinal part divides aerial parts and under ground portion.To zones of different, Various Seasonal, different year, content and the weight of different aerial partss and under ground portion are measured, and have determined the ingredient proportion of aerial parts under ground portion, and result is as follows:
(1) Herba Houttuyniae aerial parts and the under ground portion of zones of different, different year are measured respectively to content, the results are shown in Table ten.
Table ten zones of different Herba Houttuyniae aerial parts and under ground portion content results
Figure BDA0000108687760000111
Figure BDA0000108687760000121
Annotate: component A:4-methyl isophthalic acid-isopropyl-3-cyclohexene-1-alcohol
B component: 2-(4-methyl-3-cyclohexenyl group) isopropyl alcohol
Component C: borneol acetate
Component D: methylnonanone
Above result shows: Herba Houttuyniae under ground portion four constituent contents of zones of different are all higher than the content of aerial parts; Biennial under ground portion four constituent contents are higher than annual under ground portion content; Annual aerial parts four constituent contents will be higher than biennial aerial parts; Four constituent contents with regional aerial parts differ greatly, but the content difference of under ground portion is less, relatively stable.
(2) Various Seasonal Herba Houttuyniae aerial parts and under ground portion are measured respectively to content, the results are shown in Table 11.
The content results of table ten a Various Seasonal Herba Houttuyniae ground, under ground portion
Figure BDA0000108687760000122
Above result shows: Herba Houttuyniae under ground portion four constituent contents of Various Seasonal are all higher than the content of aerial parts.The content difference of Various Seasonal aerial parts is larger, but the content difference of under ground portion is less, relatively stable.
(3) different times Herba Houttuyniae aerial parts and under ground portion weight:
Get Herba Houttuyniae 5 strains, weigh respectively aerial parts and under ground portion, average, and the calculated weight ratio, the results are shown in Table 12.
Table ten two Various Seasonal Herba Houttuyniae aerial partss and under ground portion weight result
Figure BDA0000108687760000123
Figure BDA0000108687760000131
Above result shows: the Herba Houttuyniae aerial parts weight of Various Seasonal all is less than under ground portion weight, and aerial parts and under ground portion weight ratio are between 1: 1 to 1: 3.
Above-mentioned research shows, because Herba Houttuyniae under ground portion content is higher than aerial parts content, Heavy Weight, and the content of Various Seasonal, zones of different is than stable uniform, and for guaranteeing different batches constant product quality homogeneous, the ingredient proportion of aerial parts and under ground portion is 1: 2 so determine.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1:
(1) booth construction: comprise the bow type of cross direction profiles or class bow type crossbeam, the horizontal bar or the cross bar that vertically distribute; Adopt long 25-30m, wide 5-6m, the transparent PVP thin film of high 3-3.5m; Girder: bamboo; Framework: steel pipe; Garden put up a shed on the ground frame, lid thin film, and form the warmhouse booth main body;
(2) plantation
1. ground, garden is prepared: select pH5.0~6.5, content of organic matter 22.78g/kg, full nitrogen is 1.19g/kg, and quick-acting potassium content is 120.32mg/kg, and available phosphorus contents is 43.63mg/kg
2. wholely: ground, the garden that will select, after (the 9-10 month) turn over ground before sowing, divide railway carriage or compartment by following distance, the wide 5-6m in railway carriage or compartment, railway carriage or compartment furrow width 1-2m, dark 0.4-0.5m, smash to pieces railway carriage or compartment face earth smooth after loose fertilise;
3. sowing: select the unblemished fish raw meat grass seeds stem with 1-2 eye, disseminate in garden on the ground by the application rate of 40-50kg/ mu; Then earthing, thickness of earth-fill cover generally are advisable with the 10-15cm left and right; All can sow the whole year;
4. overlay film time: directly put up plastic sheeting or put up again in several days after sowing finishes;
(3) management
1. thermoregulation is controlled: budding time (till namely sending out 1-2 bud to each kind stem after the plantation),, in ground, garden plantation layer, daytime temperature is controlled at 20-25 ℃ of scope; After this cool the temperature to 20 ℃;
2. irrigate: Herba Houttuyniae belongs to moisture loving plant, therefore on ground, whole trophophase garden, will keep soil moisture to be greater than 75%, generally waters 3-5 time;
3. topdress: in neat seedling stage, the farm manure become thoroughly decomposed of use is carried Seedling, every mu of 1000-1500kg, during fertilising, every mu separately adds carbamide 15-20kg, nitrogen, phosphorus, K composite fertilizer 5-8kg, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16: 15 or 16: 15 or 16, dissolve in wherein and apply in the lump; Stem, leaf vigorous period (mid-May-to mid-June), every mu of farm manure 1000-1500kg that executes to become thoroughly decomposed, during fertilising, every mu separately adds carbamide 10-12kg and dissolves in wherein and apply in the lump;
4. weeding: weeds, with seeing with removing, avoid striving rich water with Seedling.
Embodiment 2:
(1) booth construction: comprise the bow type of cross direction profiles or class bow type crossbeam, the horizontal bar or the cross bar that vertically distribute; Adopt long 25-30m, wide 5-6m, the transparent PVP thin film of high 3-3.5m; Girder: bamboo; Framework: steel pipe; Garden put up a shed on the ground frame, lid thin film, and form the warmhouse booth main body;
(2) plantation
1. garden ground is prepared: execute well-rotted farmyard manure barnyard manure, compost or make compost 1000-1500kg and nitrogen, phosphorus, K composite fertilizer 100-150kg for every mu, wherein nitrogen, phosphorus, potassium mass ratio are 15: 16: 16;
2. wholely: the ground, garden that will select, after before sowing, being turned in ground, divide railway carriage or compartment by following distance, the wide 5-6m in railway carriage or compartment, railway carriage or compartment furrow width 1-2m, dark 0.4-0.5m, smash to pieces railway carriage or compartment face earth smooth after loose fertilise; 3. sowing: select the unblemished fish raw meat grass seeds stem with 1-2 eye, disseminate in garden on the ground by the application rate of 40-50kg/ mu; Then earthing, thickness of earth-fill cover generally are advisable with the 10-15cm left and right;
4. overlay film time: directly put up plastic sheeting or postpone and putting up again in several days after sowing finishes;
(3) management
1. thermoregulation is controlled: budding time (till namely sending out 1-2 bud to each kind stem after the plantation),, in ground, garden plantation layer, daytime temperature is controlled at 20-25 ℃ of scope; After this cool the temperature to 20 ℃;
2. irrigate: Herba Houttuyniae belongs to moisture loving plant, therefore on ground, whole trophophase garden, will keep soil moisture to be greater than 75%, generally waters 3-5 time;
3. topdress: in neat seedling stage, the farm manure become thoroughly decomposed of use is carried Seedling, every mu of 1000-1500kg, during fertilising, every mu separately adds carbamide 15-20kg, nitrogen, phosphorus, K composite fertilizer 5-8kg, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16: 15 or 16: 15 or 16, dissolve in wherein and apply in the lump; Stem, leaf vigorous period (mid-May-to mid-June), every mu of farm manure 1000-1500kg that executes to become thoroughly decomposed, during fertilising, every mu separately adds carbamide 10-12kg and dissolves in wherein and apply in the lump;
4. weeding: weeds Ying Suijian, with removing, avoids striving rich water with Seedling.
Embodiment 3
(1) according to mass ratio, be to get 2000 kilograms, the fresh fish raw meat grass aerial parts of embodiment 1 and Herba Houttuyniae under ground portion mixture at 1: 2, carry out vapor distillation, collect just 2000 liters of distillates, then carry out redistillation, collect 1000 liters of re-distilled liquids;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 10 minutes to dissolve, add 7 kilograms of sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization.
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
Embodiment 4
(1) according to mass ratio, be to get 2000 kilograms, embodiment 2 fresh fish raw meats grass aerial partss and Herba Houttuyniae under ground portion mixture at 1: 3, carry out vapor distillation, collect just 1500 liters of distillates, then carry out redistillation, collect 850 liters of re-distilled liquids;
(2) to adding weight/volume in re-distilled liquid, being 2.9 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 8 minutes to dissolve, add 7 kilograms of sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization.
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.

Claims (10)

1. the preparation method of a cordate houttuynia eye drops, is characterized in that, the method comprises the steps:
(1) according to mass ratio, be that 1:1-3.5 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 1000-3000 parts by volume, then carry out redistillation, collect re-distilled liquid 700-1300 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰-3 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops;
Herba Houttuyniae in the method refers to the Herba Houttuyniae of greenhouse gardening, and greenhouse gardening comprises the steps:
(1) booth construction: comprise the bow type of cross direction profiles or class bow type crossbeam, the horizontal bar or the cross bar that vertically distribute; Adopt long 25-30m, wide 5-6m, the transparent PVP thin film of high 3-3.5m; Girder: bamboo; Framework: steel pipe; Garden put up a shed on the ground frame, lid thin film, form the warmhouse booth main body;
(2) plantation
Ground, garden is prepared: select pH5.0~6.5, content of organic matter 20-25g/kg, full nitrogen is 1.0-1.5g
/ kg, quick-acting potassium content are 100-150mg/kg, and available phosphorus contents is the sandy loam of 40-50mg/kg;
Whole ground: the ground, garden that will select, after before sowing, being turned in ground, divide ,Ji railway carriage or compartment, railway carriage or compartment wide 5-6m by following distance, railway carriage or compartment furrow width 1-2m, dark 0.4-0.5m, smash to pieces railway carriage or compartment face earth smooth after loose fertilise;
Sowing: select the unblemished fish raw meat grass seeds stem with 1-2 eye, disseminate in garden on the ground by the application rate of 40-50kg/ mu; Then earthing, thickness of earth-fill cover is advisable with 10-15cm; Annual sowing;
The overlay film time: directly put up plastic sheeting or postpone and putting up again in several days after sowing finishes;
(3) management
Thermoregulation is controlled: budding time,, till namely after the plantation, sending out 1-2 bud to each kind stem, in ground, garden plantation layer, daytime temperature is controlled at 20-25 ℃ of scope; After this cool the temperature to 20 ℃;
Irrigate: will keep soil moisture to be greater than 75% to whole trophophase garden, water 3-5 time;
Topdress: in neat seedling stage, carry Seedling, every mu of 1000-1500kg with the farm manure become thoroughly decomposed, during fertilising, every mu separately adds carbamide 15-20kg, nitrogen, phosphorus, K composite fertilizer 5-8kg, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16:15 or 16:15 or 16, dissolve in wherein and apply in the lump; Stem, leaf vigorous period be mid-May to mid-June, every mu of farm manure 1000-1500kg that executes to become thoroughly decomposed, during fertilising, every mu separately adds carbamide 10-12kg and dissolves in wherein and apply in the lump;
Weeding: weeds, with seeing with removing, avoid striving rich water with Seedling.
2. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:2 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 10 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
3. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:3 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 1500 parts by volume, then carry out redistillation, collect re-distilled liquid 850 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.9 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 8 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
4. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:1.5 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2500 parts by volume, then carry out redistillation, collect re-distilled liquid 1300 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.6 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 15 minutes to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
5. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:2 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.7 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
6. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:2 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.9 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
7. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:2 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 3 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
8. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:1.5 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(after the cleaning of (3) eye-drop liquid bottle, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
9. the preparation method of cordate houttuynia eye drops as claimed in claim 1, is characterized in that the method comprises the steps:
(1) according to mass ratio, be that 1:2.5 gets fresh fish raw meat grass aerial parts and Herba Houttuyniae under ground portion mixture 2000 weight portions, carry out vapor distillation, collect just distillate 2000 parts by volume, then carry out redistillation, collect re-distilled liquid 1000 parts by volume;
(2) to adding weight/volume in re-distilled liquid, being 2.5 ‰ polyoxyethylene sorbitan monoleate, stirring and made in 5-20 minute to dissolve, add 7 weight portion sodium chloride, stirs and made in 10 minutes to dissolve, is 5.0-6.0 with 10% citric acid soln adjusting pH value;
(3) after eye-drop liquid bottle cleans, dry with ozone sterilization;
(4) to the re-distilled liquid after step (2) processing, use the filter element of 0.45 μ m and 0.22 μ m to filter, embedding becomes 5ml, 10ml, obtains cordate houttuynia eye drops.
10. as the preparation method of the arbitrary described cordate houttuynia eye drops of claim 1-9, it is characterized in that in the method garden be prepared as: content of organic matter 20-25g/kg, full nitrogen is 1.0-1.5g/kg, and quick-acting potassium content is 100-150mg/kg, and available phosphorus contents is 40-50mg/kg; Before ground, described garden is prepared to refer to sowing, execute well-rotted farmyard manure barnyard manure, compost or make compost 1000-1500kg and nitrogen, phosphorus, K composite fertilizer 100-150kg for every mu, wherein nitrogen, phosphorus, potassium mass ratio are 15 or 16:15 or 16:15 or 16; The described overlay film time is before temperature is reduced to 15 ℃.
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