JP3681210B2 - Method for producing rich and flavored fish soy sauce and fish flavored and soy sauce obtained by the production method - Google Patents

Method for producing rich and flavored fish soy sauce and fish flavored and soy sauce obtained by the production method Download PDF

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Publication number
JP3681210B2
JP3681210B2 JP02616696A JP2616696A JP3681210B2 JP 3681210 B2 JP3681210 B2 JP 3681210B2 JP 02616696 A JP02616696 A JP 02616696A JP 2616696 A JP2616696 A JP 2616696A JP 3681210 B2 JP3681210 B2 JP 3681210B2
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Japan
Prior art keywords
soy sauce
fish
rich
flavor
fish soy
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JP02616696A
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JPH09191850A (en
Inventor
信彦 堂本
吉富  文司
鏗 智 王
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Nippon Suisan KK
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Nippon Suisan KK
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Description

【0001】
【産業上の利用分野】
この発明は濃厚で風味の改良された魚醤油の製造法およびその製造法で得られた濃厚で風味の改良された魚醤油に関する。詳細にはこの発明はエクストルーダによって加圧、加熱、膨化処理した醸造原料により製麹することを特徴とする風味の改良された魚醤油の製造法およびその製造法で得られた濃厚で風味の改良された魚醤油に関する。
【0002】
【従来の技術】
ニョクマム、ナンプラーに代表される魚醤油は魚介類原料に食塩を20〜30%程度添加して樽などに漬け込み、1年〜2年間放置するだけで魚介類由来の自己消化酵素の作用により蛋白質が分解されエキスとなる。このエキス分をろ過して残さを除き、さらに火入れした後、沈殿物および浮遊物を除去する方法により製造されている。
【0003】
この方法によって作られる魚醤油は独特のうまみを持っているが、魚介類特有の生臭さや油臭さおよび腐敗菌の作用によって生じる腐敗臭が特徴である。そこで魚介類を原料として有用微生物を利用して製麹を行い、魚介類に特有の良好な風味を有し、しかも魚介類が持つ生臭さなどのない液体調味料を得ようとする試みが種々行われている。
【0004】
例えば特開昭53−66499号公報には魚介類原料よりエキス分を浸出除去した浸出残さ、例えばフィッシュミール、カツオ節のだし浸出残さ、あるいは煮干浸出残さなどに麦類、米類などの炭水化物原料を加え、次いでこれにアスペルギルスソーヤ等の麹菌を接種、培養し、酵母添加したものを加熱処理する方法が示されている。
【0005】
また、特公昭60−3463号公報にはフィッシュミールにデンプン粉末を混合して蒸煮し、これに糸状菌、例えばアスペルギルスソーヤ等の醤油麹菌を接種して製麹し、その魚麹に食塩による防腐環境下でさらに酵母を添加して発酵させることにより、調味素材を製造する方法が開示されている。
さらに、特開平4−325084号公報には、魚粉にアスペルギルス・グラウカスを接種し、魚粉を水分含有量20〜28%の低水分に調整し、その魚粉を30℃の温度に2日以上保持して麹菌を繁殖させ魚麹を製造した後発酵、熟成して魚醤を製造する方法が開示されている。
そして、特開平7−163310号公報には生鮮魚介類に麦類などの炭水化物原料を加えて、水分含量を調整した後、アスペルギルマ、タマリ等の麹菌を接種、培養し、発酵・熟成させる方法が示されている。
【0006】
【発明が解決しようとする課題】
特開昭53−66499号公報や特公昭60−3463号公報や特開平7−163310号公報や特開平4−325084号公報に開示されている方法は、大豆から作られる一般的な醤油と同様に麹菌の糸状菌を利用することにより、魚特有の不快臭を除去しようとするものである。
しかしながら、上記の4法では 、原料処理過程及び/または製麹過程において微生物管理の問題、原料特有の風味の保持において問題がある。その解決のためには高度な設備と管理が要求される。
【0007】
【課題を解決するための手段】
この発明では魚介類と炭水化物原料を単時間に加圧、加熱、膨化処理を後った後製麹し、発酵、熟成させ、魚醤油を製造するようになった。
【0008】
この発明に係る魚醤油の製造方法では、魚介類を粉砕し、これと炭水化物原料を混合し、エクストルーダにて、加圧、加熱、膨化処理した醸造原料を製造する。この原料に、麹菌を接種し、20〜40℃の間で2日以上保持して、麹菌を繁殖させ麹を製造する。この麹と粉砕し熱処理した魚介類と食塩水または、この麹と食塩水さらに乳酸菌、酵母を添加してもろみとし、充分攪拌した後もろみの温度コントロールを行い、発酵、熟成させた後、搾汁、火入れ、ろ過等の処理を行って魚醤油とするのである。
【0009】
すなわち、この発明は魚醤油製造に使用する麹の醸造原料をエクストルーダによって加圧、加熱、膨化処理してから製麹し、この麹をもろみ仕込み時に食塩水かあるいは加熱処理した魚介類と混合してからさらに乳酸菌および酵母を添加し発酵、熟成させることを特徴とする魚醤油の製造法、およびその製造法で得られた魚醤油である。
【0010】
この発明で使用する魚介類は、古くから魚醤油の主要原料とされている、イカナゴ、イカ、イワシ、サバなどの多獲性魚類の肉はもちろんのこと、未利用資源として有望なオキアミ、近海アミや、水産加工廃棄物なども使用することができる。上記オキアミ(節足動物門甲殻綱軟甲亜綱ホンエビ上目オキアミ目)としては、南極オキアミが好ましいが、これに限定されない。日本近海などで漁獲されるアミ類(節足動物門甲殻綱軟甲亜綱フクロエビ上目アミ目)に属する動物も利用可能である。このようにこの発明は原料魚介類としてオキアミを使用する態様を好ましい態様として包含する。
【0011】
この発明で使用する醸造原料は炭水化物原料と動物性蛋白質原料を適度の水分の共存化、密閉系内で加圧加熱後、急激に常温下に放出する膨化処理、すなわちエクストルーダ処理を行い殺菌とともに組織を多孔質化、粗鬆化そた醸造原料である。
【0012】
この発明においては、原料魚介類を混合し粉砕するのあたっては、使用する手段は何でもよく、特に限定はないが通常の細化機、ミキサー、カッター、チョッパーが例示される。また砕片の大きさは5mm角程度以下であれば実用上支障はない。さらに、原料魚の処理も特に限定されるものではないが、沸騰水中で20〜30分処理してもよい。
【0013】
この発明で使用する麹は特に限定されない。麹は蛋白質分解酵素などの酵素および炭水化物の補給にあるから、種麹は醤油麹菌 Aspergillus sojae 、黄麹菌 Aspergillus oryzaeなどが使用可能である。また、蛋白質、炭水化物の補給の面から、蛋白質の多い魚介類と澱粉質に富む小麦、米、トウモロコシなどがよいが、蛋白質含量の高いふすまが好ましい。
【0014】
食塩は酵素分解中の防腐および耐塩性微生物の選択的増殖のために添加するが、その量は基質全体の20〜30重量%であり、その食塩濃度が約12%〜25%(W/V)になるように調整することが望ましい。
【0015】
この発明において、酵素、熟成のために使用する耐塩性微生物は特に限定されない。例えば、耐塩性酵母(Zygosaccharomyces rouxxii,Torulopsis magnoliae,Torulopsis nodaensis,Torulopsis etchellsii,Torulopsis halonitratophila,Torulopsis halophila,Torulopsis mannitofaciens)などが使用される。
【0016】
このようにして、エクストルーダ処理を施した醸造原料により製麹した麹魚介類、食塩水、乳酸菌、酵母などを混合してもろみとし、充分攪拌した後、もろみを発酵タンクの中で、発酵、熟成させる。この間、原料蛋白質および炭水化物の酵素分解と耐塩性微生物による発酵、熟成作用が進行する。その際の発酵条件は通常の発酵と同じでかまわないが、特に1カ月程度15℃未満の低温下に置き、その後も20℃以下の温度で5カ月程度発酵、熟成させることが好ましい。すなわち、魚肉片および/または粗(あら)を粉砕し、これに麹、食塩水、さらに乳酸菌および酵母を添加してもろみとし、充分攪拌した後、もろみの温度コントロールを行い低温で発酵、熟成させることが好ましい。低温で発酵、熟成させた後、圧搾、火入れ、濾過等の後処理を適宜行って魚醤油とするものである。
【0017】
そして、発酵、熟成終了後、搾汁処理により液状部分が採取される。得られた濾液は、放置することにより、不溶性蛋白質などが折出し沈殿物となるので、その上清をとって生魚醤油として使ってもよい。さらに生魚醤油を加熱殺菌し、それによって出る不溶物を除いて液汁部を濾過することで、清澄な魚醤油が得られる。
【0018】
上記製造方法により本発明は風味、香り、性状において、従来の魚醤油の独特の不快臭を改善した濃厚な味の魚醤油を製造することができる。
【0019】
【実施例】
本願発明の詳細を実施例で説明する。本願発明はこれら実施例によって何ら限定されるものではない。
【0020】
実施例1
近海アミ10kgをサイレントカッターで微粉砕した。これとふすまを1:1の割合で混合し、10kg/cm2、110℃でエクストルーダ処理した。このアミとふすまによる醸造原料に1/1000のA−sojaeを添加し、よく混合後、品温を25〜35℃に保ちながら2日間製麹した。この麹3kgと20分間ボイル処理したアミ7.5kgと食塩水4.5kgを混合した。この混合物に耐塩性乳酸菌と酵母を20:1の割合で添加し、15℃未満で1カ月以上静置した。その後20℃未満の温度で4カ月程度発酵、熟成させた後、もろみを搾汁、火入れ、濾過することにより全窒素が2.4〜2.8%を示し、芳醇な香りと濃厚な旨みを合わせ持つ魚醤油11.0kgが得られた。
【0021】
比較例1
オキアミ7.5kgをサイレントカッターで微粉砕した後沸騰するまで加熱して20分間ボイルした。冷却後、食塩1.5kgを添加して混合し7日間5℃に保管し塩とオキアミを馴染ませた後、小麦麹3kgを添加し混合した。この混合物に耐塩性乳酸菌と酵母を15:1の割合で添加し、15℃未満の低温で1カ月以上静置した。その後20℃未満の温度で4カ月程度発酵、熟成した後、もろみを搾汁、火入れ、濾過することにより、全窒素が1.5〜1.9%の清澄な濾液、10.5kgを得た。
【0022】
比較例1および実施例1で得られたNaCl濃度16%の魚醤油を4倍に希釈し、よく訓練された官能検査パネル15名を用い、比較例のサンプルの評価を0点とした時の実施例1のサンプルを−4〜+4点の順位法により評価した。
その結果を表1に示す。
【0023】
【表1】

Figure 0003681210
【0024】
表から判るようにエクストルーダにより原料処理した実施例では、単にボイルしただけの比較例1に比べて明らかに高い評価がなされている。その原因として、香りの点では、原料の加熱処理が密閉高圧下で短時間に行われたことが上げられる。また味の点では、比較例に比べて実施例の方が原料のアミの使用量が多いことと、加圧、加熱、膨化処理しているために酵素消化されやすい形状にアミタンパクが変化していることが上げられる。
これらのことから、従来の魚醤油の不快臭が全くない甘い香りと濃厚な味を持つ優れた品質の魚醤油であることが裏付けられた。
【0025】
【発明の効果】
魚介類原料より、従来の不快臭の全くない、濃厚で芳醇な魚醤油を製造することができる。[0001]
[Industrial application fields]
The present invention relates to a method for producing a thick and flavor-enhanced fish soy sauce, and a fish sauce that is obtained by the production method and has a rich and improved flavor. Specifically, the present invention relates to a method for producing a fish soy sauce with improved flavor, characterized in that it is made by brewing raw material that has been pressurized, heated and expanded by an extruder, and a rich and improved flavor obtained by the method. Related to fish soy sauce.
[0002]
[Prior art]
Fish soy sauce represented by Nyokumam and Nampula is made by adding 20-30% salt to seafood ingredients, soaking them in barrels, etc., and leaving them for 1 to 2 years. Decomposed into extract. The extract is filtered to remove the residue, and after burning, the precipitate and suspended matter are removed.
[0003]
Fish soy sauce made by this method has a unique umami, but is characterized by the raw odor and oily odor unique to seafood and the rot odor produced by the action of spoilage bacteria. Therefore, various attempts have been made to produce liquid seasonings that have a good flavor peculiar to seafood and that do not have the raw odor of seafood. Has been done.
[0004]
For example, in JP-A-53-66499, carbohydrate raw materials such as wheat and rice are added to a leach residue obtained by leaching and removing an extract from a seafood raw material, such as fish meal, bonito soup leach, or boiled leach residue. In addition, a method of inoculating and cultivating koji molds such as Aspergillus soya, culturing, and heat-treating the yeast added thereto is shown.
[0005]
In Japanese Patent Publication No. 60-3463, fish meal is mixed with starch powder, cooked, inoculated with fungi, for example, soy sauce koji mold such as Aspergillus soja, and the fish cake is preserved with salt. A method for producing a seasoning material by adding yeast and fermenting under an environment is disclosed.
Furthermore, in Japanese Patent Laid-Open No. 4-325084, fish meal is inoculated with Aspergillus glaucus, the fish meal is adjusted to a low moisture content of 20 to 28%, and the fish meal is kept at a temperature of 30 ° C. for 2 days or more. A method for producing fish soy by fermenting and aging after producing koji molds by breeding koji molds is disclosed.
JP-A-7-163310 discloses a method in which a carbohydrate raw material such as wheat is added to fresh fish and shellfish, and after adjusting the water content, inoculated and cultured with Aspergillus, Tamari and other koji molds, fermented and matured. It is shown.
[0006]
[Problems to be solved by the invention]
The methods disclosed in JP-A-53-66499, JP-B-60-3463, JP-A-7-163310, and JP-A-4-325084 are the same as general soy sauce made from soybeans. It is intended to remove the unpleasant odor peculiar to fish by utilizing filamentous fungi of Aspergillus oryzae.
However, the above four methods have a problem of microorganism control in the raw material treatment process and / or the koji making process, and a problem in maintaining the flavor peculiar to the raw material. To solve the problem, advanced equipment and management are required.
[0007]
[Means for Solving the Problems]
According to the present invention, fish and soy sauce and carbohydrate raw materials are subjected to pressurization, heating, and expansion in a single hour, and then subjected to koji making, fermentation and ripening to produce fish soy sauce.
[0008]
In the method for producing fish soy sauce according to the present invention, seafood is pulverized, this is mixed with a carbohydrate raw material, and a brewing raw material that has been pressurized, heated, and expanded by an extruder is produced. The raw material is inoculated with koji mold and kept at 20 to 40 ° C. for 2 days or more to propagate the koji mold and produce koji. After mashing and heat-treating fish and shellfish and salt solution, or mash and salt solution, lactic acid bacteria and yeast are added to the mash, and after sufficient stirring, the temperature of the mash is controlled, fermented and matured, and then squeezed The fish soy sauce is processed by burning, filtering and the like.
[0009]
That is, the present invention is to make a koji brewing raw material used in fish soy production by pressurizing, heating, and expanding with an extruder, and then mixing the koji with salted water or heat-treated fish and shellfish at the time of mashing. A method for producing fish soy sauce characterized by further adding lactic acid bacteria and yeast, followed by fermentation and ripening, and fish soy sauce obtained by the production method.
[0010]
The seafood used in the present invention has long been the main raw material for fish soy sauce, as well as meat from high-capacity fish such as squid, squid, sardines, mackerel, as well as krill and near sea that are promising as unused resources Ami and fishery processing waste can also be used. As the krill (arthropod phylum crustacea soft subclass hon shrimp upper krill), Antarctic krill is preferable, but is not limited thereto. It is also possible to use animals belonging to the mysids (arthropods, crustaceans, crustaceans, submarine lobsters) that are caught in the waters near Japan. Thus, this invention includes the aspect which uses krill as raw material seafood as a preferable aspect.
[0011]
The brewing raw material used in this invention is a saponification and sterilization by exfoliation processing, that is, extruding treatment, that is, a carbohydrate raw material and an animal protein raw material coexisting in an appropriate amount of water, and pressurizing and heating in a closed system, and then rapidly releasing to normal temperature. Is a porcelain and porosification raw material.
[0012]
In this invention, when mixing and crushing raw fish and shellfish, any means may be used, and although there is no particular limitation, a normal thinning machine, mixer, cutter and chopper are exemplified. If the size of the fragments is about 5 mm square or less, there is no practical problem. Furthermore, the treatment of the raw fish is not particularly limited, but may be treated in boiling water for 20 to 30 minutes.
[0013]
The soot used in the present invention is not particularly limited. Since koji is used to supplement enzymes such as proteolytic enzymes and carbohydrates, soy sauce koji Aspergillus sojae and yellow koji Aspergillus oryzae can be used as seed koji. From the viewpoint of protein and carbohydrate supplementation, fish and shellfish rich in protein and wheat, rice and corn rich in starch are preferred, but bran having a high protein content is preferred.
[0014]
Sodium chloride is added for preservative and salt-tolerant microorganisms during enzymatic degradation, but the amount is 20-30% by weight of the total substrate, and the salt concentration is about 12-25% (W / V It is desirable to adjust so that.
[0015]
In the present invention, the enzyme and the salt-resistant microorganism used for aging are not particularly limited. For example, salt-tolerant yeasts (Zygosaccharomyces rouxxii, Torulopsis magnoliae, Torulopsis nodaensis, Torulopsis etchellsii, Torulopsis halonitratophila, Torulopsis halophila, Torulopsis mannitofaciens) are used.
[0016]
In this way, koji fish and shellfish, salt solution, lactic acid bacteria, yeast, etc., made from the brewing material that has been subjected to the extruder treatment, are mixed into a mash, and after sufficient stirring, the mash is fermented and aged in a fermentation tank. Let During this time, enzymatic degradation of raw protein and carbohydrate and fermentation and ripening by salt-resistant microorganisms proceed. Fermentation conditions at that time may be the same as those for normal fermentation, but it is particularly preferable to place them under a low temperature of less than 15 ° C for about 1 month, and then to ferment and mature at a temperature of 20 ° C or less for about 5 months. In other words, smash fish pieces and / or crude, add mash, salt solution, lactic acid bacteria and yeast to the mash, stir well, control the temperature of the mash, and ferment and mature at low temperature It is preferable. After fermenting and aging at a low temperature, fish soy sauce is obtained by appropriately performing post-treatments such as pressing, burning, and filtration.
[0017]
And a liquid part is extract | collected by a squeezing process after completion | finish of fermentation and ageing | curing | ripening. When the obtained filtrate is allowed to stand, insoluble proteins and the like are shed and become a precipitate, and the supernatant may be taken and used as raw fish soy sauce. Furthermore, a fresh fish soy sauce is obtained by heat-sterilizing raw fish soy sauce and filtering the soup part by removing the insoluble matter produced thereby.
[0018]
By the said manufacturing method, this invention can manufacture the fish sauce of the rich taste which improved the peculiar unpleasant odor of the conventional fish soy sauce in flavor, aroma, and a property.
[0019]
【Example】
The details of the present invention will be described in Examples. The present invention is not limited to these examples.
[0020]
Example 1
10 kg of near-sea honey was finely pulverized with a silent cutter. This and bran were mixed at a ratio of 1: 1 and subjected to an extruder treatment at 10 kg / cm @ 2 and 110.degree. 1/1000 A-sojae was added to the raw material for brewing with this koji and bran, and after mixing well, koji was made for 2 days while keeping the product temperature at 25 to 35 ° C. 3 kg of this koji, 7.5 kg of honey boiled for 20 minutes, and 4.5 kg of saline were mixed. To this mixture, salt-tolerant lactic acid bacteria and yeast were added at a ratio of 20: 1, and the mixture was allowed to stand at 15 ° C. or lower for one month or longer. After fermentation and aging at a temperature of less than 20 ° C for about 4 months, the mash is squeezed, fired, and filtered to show 2.4 to 2.8% of total nitrogen, with a rich fragrance and rich umami. 11.0 kg of fish soy sauce was obtained.
[0021]
Comparative Example 1
After 7.5 kg of krill was pulverized with a silent cutter, it was heated until boiling and boiled for 20 minutes. After cooling, 1.5 kg of sodium chloride was added and mixed, and stored at 5 ° C. for 7 days to adjust the salt and krill, and then 3 kg of wheat bran was added and mixed. To this mixture, salt-tolerant lactic acid bacteria and yeast were added at a ratio of 15: 1 and allowed to stand at a low temperature of less than 15 ° C. for 1 month or longer. Then, after fermentation and ripening at a temperature of less than 20 ° C. for about 4 months, the mash was squeezed, fired and filtered to obtain a clear filtrate with 1-5 kg of total nitrogen of 1.5 to 1.9%. .
[0022]
When the fish soy sauce having a NaCl concentration of 16% obtained in Comparative Example 1 and Example 1 was diluted 4-fold, 15 well-trained sensory test panels were used, and the evaluation of the sample of the comparative example was 0 point. The sample of Example 1 was evaluated by a ranking method of -4 to +4 points.
The results are shown in Table 1.
[0023]
[Table 1]
Figure 0003681210
[0024]
As can be seen from the table, the examples in which the raw materials were processed by the extruder were clearly evaluated highly as compared with the comparative example 1 which was simply boiled. The reason for this is that, in terms of fragrance, the heat treatment of the raw material was performed in a short time under a closed high pressure. In addition, in terms of taste, the example uses a larger amount of the raw material, compared to the comparative example, and the amino acid changes into a shape that is easily digested by the enzyme because it is pressurized, heated, and expanded. Is raised.
From these facts, it was proved that the fish soy was of excellent quality having a sweet scent and a rich taste without any unpleasant odor of conventional fish soy sauce.
[0025]
【The invention's effect】
From fish and shellfish raw materials, it is possible to produce a thick and rich fish soy sauce without any conventional unpleasant odor.

Claims (8)

魚醤油の製造において、未処理の魚介類を原料とし、粉砕した該魚介類と炭水化物原料を混合し、エクストルーダによって加圧、加熱、膨化処理して製造した醸造原料により製麹することを特徴とする濃厚で風味の改良された魚醤油の製造法。In the production of fish soy sauce, untreated fish and shellfish are used as raw materials, the ground fishery products and carbohydrate raw materials are mixed, and the mixture is subjected to pressurization, heating and expansion treatment with an extruder, and the koji is made from the brewing raw material. To make fish soy sauce with rich flavor. もろみ仕込み時に魚介類に食塩および麹を加えてから、さらに乳酸菌および酵母を添加し、その後、もろみを発酵熟成させる請求項1の濃厚で風味の改良された魚醤油の製造法。2. The method for producing a thick and flavorful fish soy sauce according to claim 1, wherein salt and straw are added to the seafood at the time of mash preparation, lactic acid bacteria and yeast are further added, and then the mash is fermented and matured. 魚介類として甲殻類を使用する請求項1または2の濃厚で風味の改良された魚醤油の製造法。3. A method for producing a thick and flavored fish soy sauce according to claim 1 or 2, wherein crustaceans are used as seafood. 乳酸菌および酵母として耐塩性乳酸菌および耐塩性酵母を使用する請求項2または3の濃厚で風味の改良された魚醤油の製造法。4. The method for producing a thick and flavor-rich fish soy sauce according to claim 2 or 3, wherein salt-resistant lactic acid bacteria and salt-resistant yeast are used as lactic acid bacteria and yeast. 乳酸菌の添加量を酵母の添加量の10倍以上の割合で添加する請求項2、3または4の濃厚で風味の改良された魚醤油の製造法。The method for producing a thick and flavor-rich fish soy sauce according to claim 2, 3 or 4, wherein the addition amount of lactic acid bacteria is added at a ratio of 10 times or more of the addition amount of yeast. もろみの発酵・熟成を低温で行う請求項1ないし5のいずれかの濃厚で風味の改良された魚醤油の製造法。The method for producing fish soy sauce having a rich flavor and improved flavor according to any one of claims 1 to 5, wherein moromi is fermented and matured at a low temperature. もろみの低温発酵・熟成がもろみ仕込み時から1ヶ月以上15℃未満に保持し、その後20℃未満の温度で低温長期間発酵・熟成させることである請求項6の濃厚で風味の改良された魚醤油の製造法。7. The fish having a rich flavor and improved flavor according to claim 6, wherein the low temperature fermentation and ripening of moromi is maintained at a temperature of less than 15 ° C for at least 1 month from the time of mashing, and then fermented and ripened at a temperature of less than 20 ° C for a long period of time. Soy sauce production method. 請求項1ないし7のいずれかの製造法で得られた濃厚で風味の改良された魚醤油。A fish soy sauce having a rich and improved flavor obtained by the production method according to any one of claims 1 to 7.
JP02616696A 1996-01-19 1996-01-19 Method for producing rich and flavored fish soy sauce and fish flavored and soy sauce obtained by the production method Expired - Fee Related JP3681210B2 (en)

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