DE1927996A1 - Stable, concentrated hop preparation and process for its production - Google Patents

Description

The invention "hits" in a stable, consistent hop preparation eowle the process ma 8tlntr Htrtttllunig ·

BTI dtr BitrbanrttOLlme fladtt dlt Yirwnflung fön Eaptmtkoo "9xrmi _$ WjLt * .B, ft1n4ttb1twf hop on Bitttretoff engtrtloiiertttk pttlTtrfttralgtM Hoyf" t OTDR Hopfjjtotxtmkt order * r grü-vr · distribution. Dl · Yorttll «gtetnüber Vaturhopf tu btstthtn Tor everything - with hop extract In the much smaller volume, the lower weight and in the berry possibility of an airtight packaging, which means that the shelf life and storability are significantly increased. Furthermore, this froductea tine reaches very or less pronounced detriment of the outside solution of the hop bitter substances. Am part dieeer "Hopfenkoneerren" la PulTerfor · is offered, while Hopfeoextrakt in foxm a paste Torliect, dlt at Teaperaturen about 60 ⁰ C au 'ine' thin 'syrup ftoeailst.

Duroh dl uterführung in dit the most complete bowl can preserve

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V *

weekly bitter ingredients for brewing beer per oe * wlohteeinheit an hops bsw «, Hopfenpxmparat on daa oa · awelfaone with enriched hop powder, like ee e.B · under the Beselennang Hopfix is put on the market, bia auf daa dre- bla eocrhe> times with leprechaun extracts and seven times with nutritive extracts. Ia wire sweeknieeig, if nan dleaan share of head leaves dead, dead everything at a « pulYerfömigan preparation, could still increase waiter.

fieau koaart, that the individual Beatand parts dea flopfena, which are considered for the beer production ala weekly, also the bitter ingredient elnereeita and the hop tannin andararaeita, rwe would require a long Xoohaeiten, to your —Tina! While the hop tannins, of which it is generally narrowed that they are unarlftaalieh on a good turbulence in the brewing process, require a cloak of τοη mlndeatena in two positions, on "and good trotting, will help the sweetening cohesion of the bitter ingredient content not only - waa gewttnaoht let - transferred into the aigentliea bitter onea Of-Sftaren, aondam ea also aehon a certain degradation atatt · If the bitter ingredient a wire alao a Jtooheeit ▼ ona ) bia nucbaten If there were optlweu for the aranatlBierung dea Biera, which is largely caused by the hop owls, the soohaeit »ögliöhat YK hour should not be tiberaohreiten, since the Hopfeaöl · vaaeeitlaw ^ filuchtlg aladl and aoait e very quick escape ·

In the case of enriched hop palTera liagaai dleae leateiwiteile atata geatUeea W ₉ ao dal in the case of the Blerheratcllveg old angarai-

SopfenfalTer, abenao as in TanreniMig voi ran in ee Partlea emgagabea, and Fextle «a tagt— *** fi» ohung, who laegiiaaal bla sm t

m 2 ~

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BATH ORIGINAL

is boiled in order to bring about a good turbulence, a further batch after about YZ to 1 hour, in which the bitter substances should take place, and a third batch towards the end of the boiling, which is to serve for flavoring, because the remaining is short Reetkochzeit there is still a sufficient amount of hops ·· oil left.

When using hop extract, this could be a disadvantage generally switched off, because here through the production conditionally there may be tractions, namely predominantly ouch Bitteratoff existing solvent extract and the tannins Containing · aqueous extract · Since hop tannin alone is often used is not durable, but if stored for a long time, especially at the higher temperatures that occur in the tropics, it leads to gas development and bombing of the cans, but on the other hand - as already mentioned - the presence of hops tannin is essential for cooking the cloud formation is considered, "bitter substance and hop tannin are mixed up and la marketed in this form ",

Therefore Bs would also hig radig erwUnecht when nan would grouting a stable hop preparation which contains depending on the desired Vervendun ^ amweck Hopfenbitteretoff, Hopfengerbetoff or a mixture of the two, so the entire Hopfeninhalteetoffe "

The object of the present invention is therefore a powdery egg Hopf enprmparat, which can also be used at elevated temperatures for a longer period of time Period of time is stable 1st, and if desired, hop leaf matter, Contains hops tanning agent or both components

It has now been found that this is possible by means of a stable, concentrated hop preparation which consists of an intimate mixture of

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fine outer silica and hop extract or hop extract proportions ordered "

The small amounts of cleaeloure to hop extract or Hop extract proportions are preferably 0.25 to I ^ inebee.

0.3 to 0.6 parts of silica to 1 part of hop extract or hop extract proportions.

Under hop extract let not only the so-called «8tendardextrakt- su understand the Hopfenbitteretoffe and -gerbstoffe aufweint in dexn in na" türlichtm hop Torkomenden Yerhältnls, eondern arbitrarily · Mi # ohun {; s of these two £ aaponenten _o put under hops extract "" are either fiopfenbltter "toff (Löeongeeittelextraki;) or" r Hopfeee "rbetoffe (" fiJBrl ^ er AuMiug) or any lntelle darroo κα recrstehec "

De. "Ioh through the transfer into powdered extracts with sub-

1 _

Klkroekopisca finely divided silicic acid hops bitter extract and tanning agent "xtrncts not only geaeinea *, but can also be produced separately in a holding fora, there is now the option of bittering hops off and hops bittering substance % u any" desired point of view can be suspended. Pre-boil every 1 hour old hop fermentation material for protein precipitation and then only add the hop bittering agent and continue to boil for 1 hour. This ensures both sufficient turbidity and sufficient isomerization, but without degradation by excessive coals.

The process for the production of this stable, enriched hopsprfiperate consists in that one extracts Uop extract or hop extract parts, aweckBäeeig in solution or ijuapenslon, with finely divided silica ElseM and cagebcoaexifaXle rorhandesi ·· Löeutigeelttel or dispersion medium.

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BATH ORIGINAL

becomes the hops extract or the hop extract fraction

in a layer of the fefxx distributed silica

gerökrfe oral axisclslieeseral the heat is stirred into silica.

Bas Kisefeingav-eritli.ltiiis extract ^ is zweckmäeeiger- silica, from 1: 0.3 to 0.6 Sew · grooves, wherein at hop bitter substance a MlBchatigBTeiiiältiiie wn 1 rO _t 45 _t at Hopf engerbstoff a eolahes tone. 1 £ Ö _P 4 «ßd in the case of hops cleavage extract CKiacausig aoe both) a

Vexii & itaiB van lsO _v 4 to 0.45 is varstfgt »

At. The preferential way of working of the Herat el lon ^ Bit Ιΰβαζι ^ βη ton Bopfenbltteretoff b * w »Hop tannin results, the further advantage _§ that nor less silica is needed * on a loosely rieeelfSbigeB Palrer so. Eximlten "Detdiixcii has the EDdjprodnkt iron holier bitter substance and it results in rnxxcL · eise Koetesersparni0 MneieMlich der KLeselsfture"

{iberraecBeQderweiee is dsm powderföralge hopsprparstt der Krfladung nod. "Only axtßL · the only bitter substance containing pulper" ni the powder only Serbetöffβ containing even with hßberen £ eBpei "taren beaerkenewert stable obwoltl the Hopfeninhaltsetoffe bound to a 3ubstattz Kit active surface, which expect 11βββ · _ν Dab the reduction would take place scnneller" Thus, according to the invention, there is no tendency for hops to tannin palates to κατ Bootbage ·

{iberraecneadörwelse also let the bitter substance build-up, ie the conversion of the ος acids into iso-ot acids in bitter at off powder bxw "hop extract extract of the invention" better than in the bitter substance bsw "hop extract, as the following Kurßekocirca smokes have a special character is this Torteil angereicberteat ince the Yergleiob hop powder * as * knows under the Beseicnnt ^ g "Hopfix in trade _t as also geseigt in tftirsekoohvereuchen

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Special notice! is the rapid isomerization "ie," the better the ÜBwandlung Oi acids Ib leo-Cfr Säureii mentioned in kureen cooking pages »Vie _t, it is common practice in the hops or * · the Hopfenprapexate in more Q & hen to. give · The longer cooked gifts should have a strong bitterness «the köre cooked. result in a best-planned hop arona. With longer Eochdauer the arose, schematically hop oils go volatile · The use of Hopfenbltteretoffputrer buttocks of the invention includes the naheeu ADLE hop oils, makes it possible * trota kurser Eöchzelt to give the EopfenaroMa "a good relatir Bitteretoffausnützung ta achieve"

Genes particularly surprisingly let the fact "amß" - as shown in Example 3, the Trabau "separation (protein precipitation) in the Uifrs samples cooked with hop bitter ingredients according to the test is best" This VHrsea unites Ib Qegensats do the Vtirse "samples, ie Hopf closerbetoff contain »practically clear and laeeext eich filter very well Coarse Ablämteningeseiten), Ss is therefore BÖelich, even without using τοη Hopf closerbetoff να. a good fallow image eu koBoen. Hop tannins are often used for the formation of τοη EU te turbidity in the finished beer, which represents a negative yualltäteeerkeal * Me good trubeiiesscheidun ^ If only the hop bitter substance is used, there is a contradiction to the generally recognized * fectieinnng that the hop tannins are essential for this process.

Another advantage of the BopfenpulTerpräpermtes is the Järflndung mentions that the high content of hop active ingredients, both

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epielewelse uuBgudrucks increased by CX-oHurcn, special et ark can be, as the following table zel /; t, where the ttohutt weights, the average acidic content and the OT-acid content per 100 al hops or hop preparation for two known powder » fönni / je Hopf enprii parate and two preparations according to the invention reproduced bind.

Tabel Sohiittgowloht loee pressed (X-öüure in 100 al

{, • «grind the hops

approx. b ; <■ (X-acids 2b _t l 31.5 1.3 t or 1.5 g

Enriched Hopfenyrer

10% oleic acid 30.2-30.8 43.6-44.3 3 bsw. 4-4.5 β

Hop extraJrt pulTer e

of strength 10 % O (-acids 66.6-69.6 75.4 6.6 b * v _e 7.5 g

HopbJLtteretoxTpulT «r

geeüß the Srflndniic

20 to 22 % C ^ acids 63.9-45 68.3-69.6 13 bor. 15 β

■ natural hops approx. 5 * 0f acids 3-7 20-50 n * .i-i.5 «in

Prussian hops

The enrichment gain in Qf structures, since with an enriched hop pusher compared to pressed hops, amounts to approx. 1 | 7 waa in the case of the bitter raw material pulverizer g «« ä £ the amount increased to oa · III5 «

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1927998

Another advantage of the hop preparations according to the invention is that the weight can be increased by the clover egg content, depending on the mixing ratio, to 1.4 to 1.6 with the most adequate preparations, while the well-known light powder, such as ground hops or fortified hop powder, when added to the heating pan, can easily be torn and lost with partial usage, since their specific weight is ffMHtaleiäMlf e * ri * g iat _r lat 41m btl "Hapfenpräparet Invention by increasing the specific weights by around 40 to 50 # less easy.

The following examples explain the force charge. For the following experiments a feindieperee, precipitated and spray-dried silica is used. she cheaiache 2uaasQBenset £ ung is the following:

SiO ₂ 95%, Wa ₂ O 0.8% _f SO ₅ 0.8 % _t FeO 0.05 % t BfiT surface 25Om ² Zg, pH value 6.3.

A product that is very suitable for the invention is from F *. Deguea, Hanau, available under order number K 322 . However, the silica sold under the calculation of Aerosil ^{B by} Deguea is also suitable, which gives practically the same results as further experiments have shown. Similar products are also suitable, such as equal Cieeelgel or kieselguhr.

By Kieself «! B (Merck) and for kieselguhr (Seit *, Bed Krewenach) ! Wir4 «la Terhiltnii tos 1: 0.75 to 1.25 extract su Kieeelgel

vuviem Verechiedeee vUraekochrereuche carried out ·

0098 50 /

BATH ORIGINAL

In the individual wureekochversuche was each worked identically. When comparing the various cooking tests with one another, the respective values in the absolute height due to possible different downtimes and the like differ, but Bind tends to differ jewella comparable. At four

Experiments (Vürzkochversuch 1 to 4) were each 1 1 würee with the respective preparation, which in the amount used 100 Bg ^ acids contained, boiled for 2 hours. Mach 30, 60, 90 and Ϊ20 minutes became a sample sucked and after Rigby-Bara, AiJBG-Pr9c. In 1961, when standing flat for 5 days, the wort was filtered with kieselguhr and determined again,

In the case of attempted cooking 5, 450 mg of tannin powder were cooked for 1 hour after the invention, and then 475 β hops bitter powder of the invention were sugeset, and after 30, 60 and 90 minutes, samples were sucked in. The bitter substance determination was carried out according to Rigby-Bara I and II ( ASBC Proc. 1961)

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BATH ORIGINAL

WtirsekocbfOrwach 1

a) Bitter substance control according to Rigby-Bara I (iichnelleethode)

b) Bitter substance bee timfflUJTg according to Rißty-Bare II

CM

Ch

St.

I. ■ J

4 »

fr-

tn

CVt

CQ (Λ

VO w in

CVI

O O

4 »OK

CM

tn

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CM

VO

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KV

KV

If »

kC

SO

rs

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a? ey

σι ο

»It

Hobi - Hopf «obitteretoffextrakt

Hobi-Pulrer * Hopf enbitteretoffextraJct-Pulrer ait Kl «« «l» & «rt (ßiidti

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ff

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Preparations

30 min.

Χβο-α ex

60 Hizu

90 Nl

Ιβο-α α There"

ΐ · ο-α a

after 5 days

kieselguhr

filtered

a) Bltteratoffbeatizanme naoh Rigby-Bare I (rapid method)

O I. O co CX) Oil ο
• ν. —Λ
_ * O

1000

iopfezx ·· puller

935 η «Hobi-PulT. f Tanning powder

, 5 U, 4

31.2 12.2

22.0 14.1

37.6 11.9

30.0 12.8

40.0 11.3

b) Bitterat of fbeatiamniag according to Kigby-Bare II

1000 mg Ungerelch. Iopfenipulrer

935 mn Hobi desk. + Tanning powder

18.6 11.2

20.4 10.0

19.1 11.2

24.4 8.3

21.6 9.6

28.3 7.5 35.2 12.6 45.2 13.0

26.9 11.2 33.6 8.3

33.6 5.6

40.9 5.8

25.7 4.5

28.3 4.2

All enriched Hopf egg powder was used in the Hopfix preparation.

Cooking time 30 min. Ot 17.5 10.1 60 min 90 HiBa 120 min. 22.4 8.5 29.7 CX PrÄparar -—-._ leowx a) Bi titre toffbaetiavning 30.0 9.1 Iao- (x cn Ibo-c t a Ieo- (X 33.1 7.7 36.2 1000 * g
on «enriched tea
Hopfanpulrer 24.8 10.4 naon Rigby-Bare 1 (ücimellaethode) 30.6 10.1 35.2 8.0 475 mn
Hobl-Pulrer 29.6 9.6 20.0 8.5 38.2 8.9 43.2 7.4 291 m
Hobl 31.8 8.0 9.3 970 se
Hops extract 28.6 10.1 ö, 5 34.7 9.3

sr

The Hopf Ix preparation was reserved as enriched Hopf bulky

CD C £>

WUrs «cooks« rough 5

1 1 wort «it 450 ag Gerbet offpuTrer g« aä0 of the invention 1 hour «Torc« boils and then after ingredients of 475% hops bitter powder according to the invention inageeaat 90 hours veit «rg« kooht under test numbers after 30, 60 and 90 minutes «

cooking time 30 min. OV 60 (X 90 Min. Kethode IeO- (X 12.3 I8O-0 11.2 18O- < m) 33.7 7.0 36.9 5.8 42.6 10.2 b) 19.6 21.6 24.7 6.0

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-fs'

Puffer cook ver Buchc

In 1 liter 0.1 molar phosphate buffer solution pH 5.4 the samples given in the rachfoigeisd cooked. Each Sochprobo entMel * approx. 133 mg oC

Hach 30, 60, 90 and 120 Hin. verden samples are taken and analyzed according to Rigby and Bars. For each 1 liter of buffer solution the following samples were given:

1. 400 mg head bitter substance (extract, Hallertauer 1968,

Hears company)
2 655 ng hops powder

Hop bitter extract: kieaic acid 1: 0.5)

3. 760 ng HxjCenextrakt (ratio of hop bitter ingredient:

Tanning agent -1: 1)
^. 13 * 0 ng hop extract powder (hop extract as under

specified xmü Kie8elejäure _t MiachunseverhSltnie 1: 0 _s 5)

Oa. 50 ml KcchlÖBuxig are filtered through blue ribbon and * fOO tajL Fi Itrat Biit 20 ml jtsooktane and 3 «16 nHCl There. shaken vigorously.

Then 5 nd l-cooctane extract with alk. Methanol on 25 ml filled up and measured by epectrophotometry. Calculation;

mg / 1 isohUBulon; 48 «5 * E255" * ²⁶ » ⁵ * ^E 360 * eg / l ot-ßauren: 80 ·

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After the samples had stood for five days, another Bittratoff determination was carried out. You results aind summarized in the following table.

Cooking time
preparation 30 min.
ΙβΟ-Λ <£
72.0 55.6 60. i-Iin.
leo-ck a 64.4 50.2 90
Tbq- There. 57 * 8 41.4 120 min.
leo- <* - at 45.8 After 5 Ta
gen blue
tape
filtered
ϊβο-ος »ος. 15.6 22.8 ^ a) Bitti
400 mg
Hobi ret off best im-
26.0 63.6 81.0 70.0 according to R
46.2 58.4 72.7 64.2 .gby-Barß I
57.8 51.8 62.9 52.2 (Tendon limeth
68.6 44.4 54.7 jde)
86.6 12.2 18.3 2)
I & 55 ng
Hobi-fulv. 34.5 74.8 59.2 49.5 65.9 50.2 64.4 60 ,? _
44.6 76.0 51.4 90.4 24.1 39.2 3)
760 mg
HE 27.0 • Btoffbeetimn
21.8 52.6 43.1 mg according to Hi
37.1 44.4 57.5 gby bars II
42.8 36.0 66.5 33.2 98.7 125.0 13.0 17.8 4)
1340 mg
HE-PuIv. 45.8, 27.1 63.6 41.4 76.4 57.6 86.6 34.9 68.6 1) b) Please
400 mg
Hobi 21.7 35.3 46.6 54.0 45.6 73.5 2)
655 ag
Hobi-iPulv. 33.7 48.0 60.0 69.0 37.9 72.5 54.7 85.4 19 * 0 mg
WB-TuIv. 68.7

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Example 3 ίψ

Wurakochversuche - Trubbi! dung

1 1 Würae was boiled for 2 hours each time with the preparation given in column 2 of the following table. The amount of sediment that had separated out was filtered off and dried. The nitrogen content dor Müx'.zp was determined before and after boiling. The value given under Experiment 7 for enriched hop powder also contains the spent grains from the hop preparation. * «-

It is noteworthy that the experiment 2 indicated value with hop bitter raw material powder of the refinement results in the best trub cleavage even though there is no tannin present.

Vers. Preparation Trüb IM3 «h» according to the word

(Dry weight) mg / 100 ml

0 front cube - 111.8

1,300 mg Hobl 1067 mg 106.1

2 450 mg Hobi powder. 11-90 mg 103.8

3,600 mg Ho-Extr. 1063 mg 107.7

4,900 mg Ho-Extr.-PuIv. 1057 mg 107.0 . 5 1000 ng angled hop tray. - 106.6

6,900 mg Hobi powder.

♦ Gerb.-PuIv. - 107.0

7 10 (X) mg of fermented hop powder. 1972

8,475 ng Hobi powder. 1627

9 291 mg Hobi 1-155
970 mg Ho- £ xtr.Pul, y _e 1238

In the case of Kbchvereucheia 1-6, the half of the initial and focbwurs were determined. Dia Ver ^ ic '. " 7-10 and a repetition, where n «r was the Tmu" aueg " © g" n .

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1927SSG

Example 4 μλ Manufacture of powder preparations

The powdery hop extract preparations were produced in each case using the following amount of hops extract components (Hop bitter substance and / or hop tannin) either directly or in the specified solvent with submicroscopic finely divided silica, as previously defined, mixed and, if necessary, dried as specified « When working without a solvent, the necessary amounts of silica and bitter substance were put together in the beaker with the help mixed with a spatula. A fine mixing took place afterwards in the Starmix by mixing for about 50 seconds

a) 10 g each of hop bitter ingredient (extract, Hallertauer 1960, Horst Company, Öoburg) mixed with 3, 4, 4.5, 5.6 and 10 g Silica

b) 10 g each of hop bitter substance (as above) dissolved in 10 ml of CH ₂ Cl ₂ mixed with 3, 4, 4.5, 5.6 and 10 g of silica

c) 10 g tanning agent (Hallertauer extract 1968, Horst Company, Coburg) mixed with 3, 4, 5 or 6 g of silica

d) 10 g each of hop extract (hop bitter substance: tannin «1: 1) mixed with 3» 4, 4.5, 5, 6 and 10 g of silica

e) 10 g of hop bitter substance dissolved in 50 ml of CH ₂ Cl ₂ , mixed with

5 g of silica and evaporated to dryness in a hot cation evaporator

f) 10 g of tanning agent, dissolved in 20 ml of H ₂ O, mixed with 4 g of silica and evaporated to dryness in a rotary evaporator

In series a), the lower limit for a well applicable product in the hisha ratio is 10: 4.5 ~ 5, while in Solution b) already has a mixing ratio of 10: 4.5 a fine-grained one Powder yields.

Hop extract (series d) produces a sufficiently fine-grained powder at a mixing ratio of 10: 4-4.5. In the case of tanning agents (series c), the lower grayness is 10: 4. A powder can also be obtained when added to dilute solutions (hop bitter substance 12 wt .- #, tanning agent 33 %). In the rotary evaporator, the Hasse bakes together with evaporation, but can be ground up.

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Claims (1)

• Stable kor.zanti ie / fees hop preparation, consisting of aue eirer Image * Hashing of finely divided silica and hop extract or 2. Hop preparation according to claim 1, consisting of O, 25-1, i, esp. 0.5-0.6 parts of silica to one part of hops extract or hops extract. 3 · Hop preparation according to claim 1 or 2, beet before cd & ue hop bitter; offext) react and silica. 4. Hcpf'enpräperat according to claim 1 or?, Beetehend aue Hop tan, off extract and Kieeeleäuro. 5. Hop preparation according to claim 1 or 2, beetehend aue one Mixture of hops bitter extract and hops tannin extract and pebble gel. 6. Hopferpiäparat rmch one of claims 1-5, characterized gekenoseiehnet that it contains such a silica with e ^ ncy BET surface area of about 250 m ² / g. 7 «Method of making dee stable concentrated Hop preparation according to claims 1-5, characterized in that one tute Hopfenuxtra & t or hop extract! The old fei rvert tilter silica inr.ig mixed. 8. The method according to claim 6, characterized gekencsel η c '; , dee ε one when Vcrworducg of solution-backless · First, the extract is converted into part of the silica stir in and after a homogeneous mixture has been produced, the remainder of the silica is added. 009850/1110 19279SG Process according to Claim 6, characterized in that the silica is converted into a Stir in solution or suspension of the hop extract or the hop extract portions and then removes the solvent and / or dispersant present. 10. The method according to any one of claims 6-8, characterized in that 0.3-0.6 parts Silicic acid with part T of hop extract or hop extract proportion mixed. 11. Use of the hop preparation according to claims 1-5 "- ~ ^; in the brewery. 12. Use according to claim 11 in 2 batches in the wort boiling, first of a hop tannin powder and after 30 to 90 minutes of boiling time of a hop bitter powder, 13 · Use according to claim 11 and only of hop bitter powder in wort boiling. 009850/1110 GOPY