JP2004020499A - Method of determining maturation degree of beef, and method of manufacturing mature beef using the same - Google Patents
Method of determining maturation degree of beef, and method of manufacturing mature beef using the same Download PDFInfo
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Abstract
Description
【０００１】
【発明の属する技術分野】
本発明は、牛肉の熟成度の判定方法及びそれを用いた熟成牛肉の製造方法に関する。より詳しくは、牛肉の揮発性物質を捕集した際のｎ−オクタナールを指標とした牛肉の熟成度の判定方法及びそれを用いた熟成牛肉の製造方法に関する。
【０００２】
【従来の技術】
近年の食品業界では、「おいしさ」「安全性」「簡便性」の３点が商品開発のキーワードとなっている。これまでの食品保蔵に関する研究は、腐敗の抑制及び外観の保持という「安全性」に力点が置かれてきたが、「おいしさ」に対する消費者の要求が強まる中で、”風味”を向上させる手法の研究の必要性が叫ばれはじめた。食品によっては一定条件で保蔵されることにより熟成と云う現象が起こり、味、香りと云った「おいしさ」の要素である風味が向上することが、消費者に認識されている。
おいしさへの要求が強い牛肉も一定条件で保蔵されることにより熟成という現象が起こり、味、香りと云った「おいしさ」の要素である風味が向上することが知られている。しかしながら、熟成は衛生学的に矛盾を生じやすい現象であるため、一歩間違えると腐敗につながる。また、熟成終了の判断は経験に頼っており、その判断には、熟練した技術が必要であり、客観的な基準がないのが現状である。
【０００３】
熟成度を判定する手段として、例えば特開平６−５０９６５号公報の「畜肉加工品の賞味期間の設定方法及び熟成度の判定方法」のように畜肉加工品の貯蔵臭及び特有の香気に直接関与する成分として、１，６−ジオキサシクロドデカン−７，１２−ジオンを指標とすることにより、賞味期間の設定及び熟成度の判定を可能にする方法や、特開平６−１８５１６号公報の「牛肉の熟成度測定方法」のように熟成によって増加する香気成分を測定することにより、熟成度を判定可能にする方法、また、特開平６−２６１７９２号公報の「牛肉の熟成温度履歴検知法」のように微生物を利用して熟成温度履歴を検知する方法などが開示されているが、明確な指標があっても測定のための方法が複雑であったり、明確な指標がなかったり、微生物の同定が必要であったりするため、熟成度の判定を行うのは困難であった。
【０００４】
【発明が解決しようとする課題】
本発明の目的は、簡易、且つ精度の高い牛肉の熟成度の判定方法を提供し、その判定方法を用いて美味な熟成牛肉の製造方法を提供することにある。
【０００５】
【課題を解決するための手段】
本発明者らは、牛肉の熟成度の判定を簡易、且つ精度高く行うことを鋭意検討した結果、捕集した牛肉の揮発性物質のｎ−ヘプタン、トルエン、ヘキサン酸、ｎ−オクタナール、トリメチルベンゼンが経時的に増加していることを見出し、特に和牛脂質の主要構成成分であるオレイン酸の酸化生成物質である、ｎ−オクタナールが熟成指標としてふさわしいことを見い出し、本発明を完成するに至った。
【０００６】
すなわち本発明は、牛肉の揮発性物質を捕集した際のｎ−オクタナールの濃度測定値［Ａ］とｎ−オクタナールの閾値［Ｔ］との比（α）＝［Ａ］／［Ｔ］を指標とする牛肉の熟成度の判定方法を提供する。前記発明において、（α）が０．１〜１．０の範囲のとき熟成牛肉と判定する牛肉の熟成度の判定方法を提供する。牛肉の揮発性物質を捕集した際に指標化合物として、ｎ−オクタナールを除くヘキサン酸、ｎ−ヘプタン、トルエン、及びトリメチルベンゼンから選択される少なくとも一種の化合物を含み、これらの化合物の閾値［Ｔ］ｉと対応する前記指標化合物の濃度測定値［Ａ］ｉとの比（α）ｉ＝［Ａ］ｉ／［Ｔ］ｉが、それぞれ０である前記発明の牛肉の熟成度の判定方法を提供する。また、ヘキサン酸、ｎ−ヘプタン、トルエン、及びトリメチルベンゼンから選択される少なくとも一種の化合物を含み、これらの化合物の閾値［Ｔ］ｉと牛肉の揮発性物質を捕集した際の対応する化合物の濃度測定値［Ａ］ｉとの比（α）ｉが０．０００００１〜０．０１の範囲にある前記発明の牛肉の熟成度の判定方法を提供する。更に、本発明は前記発明の牛肉の熟成度の判定方法を用いて熟成状況を判断しながら、牛肉を４０℃以下の温度条件で保存し、出荷時期を決める熟成牛肉の製造方法を提供する。
【０００７】
【発明の実施の形態】
本発明に適用可能な牛肉の種類としては、特に限定されるものではないが、例えば和牛、ホルスタイン、和牛とホルスタインを掛け合わせたＦ１などが挙げられる。熟成牛肉の製造方法は、通常、屠殺、食肉処理されて、温度０℃付近で約１４日間程度冷却されている。この段階で牛肉の熟成が行われる。熟成が済んだ肉は、整形、包装され、保管され、出荷に回される。牛肉の熟成は、流通を経て消費者の手に入る迄の時間、味とにおい及び保存の条件を考慮した経験に基づくものであった。
【０００８】
本発明者らは、熟成経過ごとの牛肉サンプルについて、内部標準としてブロモベンゼン・メタノール溶液を用い、トータルイオンガスクロマトグラムにより実施例において示した分析法により、揮発成分を分析した。代表的なピーク３５個を選び、各ピーク面積について解析し、平均値の差の検定による有意差検定を行った。３５個の物質のうち、ｎ−ヘプタン、トルエン、ヘキサン酸、ｎ−オクタナール、トリメチルベンゼンが有意差を持って経時的に増加していることを見出した。本発明では、これら５個の化合物を牛肉の揮発性物質の指標化合物と呼ぶ。また、これらの物質の閾値は、ｎ−ヘプタン２０万ｐｐｂ、トルエン５００００ｐｐｂ、ヘキサン酸３０００ｐｐｂ、ｎ−オクタナール０．７ｐｐｂ、トリメチルベンゼン５５０ｐｐｂである。なお、本発明における閾値は、ｎ−オクタナール、ｎ−ヘプタン、トルエン、ヘキサン酸、トリメチルベンゼン、いずれも水溶液濃度（重量基準）を用いる。閾値とは、ヒトがその存在を検知できる最低の濃度のことである。前記データは、ｎ−オクタナールが最も少ない濃度でもヒトの鼻では感じることを意味している。また、牛肉の揮発性物質として捕集された前記５種の指標化合物の経時変化を各々の閾値で割った値（におい指数）は、図３に示したが、この結果はｎ−オクタナールのみが、官能的に感じることを示している。
さらに、ｎ−オクタナールは、生体反応で生成し、日常の生活環境には、あまり存在しない物質である。従って、ｎ−オクタナールは、ヘプタンやトルエンのような日常の通常の環境に存在し、成熟度測定の汚染源（誤差源）となりやい物質とは異なるので、成熟度測定の指標化合物として適した物質であることがわかる。
【０００９】
本発明は、ｎ−オクタナールを牛肉の熟成の指標として熟成度の判定方法を提供するものである。該ｎ−オクタナールは、炭素８個の直鎖のアルデヒド、別名、オクチルアルデヒド、カプリルアルデヒドと呼ばれている沸点１７１〜１７３℃の無色透明の液体である。ｎ−オクタナールの香りとしては、オイリー、フルーティーとされており、オレンジ等にも含まれている。
【００１０】
本発明は、牛肉の揮発性物質を捕集した際のｎ−オクタナールの濃度測定値［Ａ］とｎ−オクタナールの閾値［Ｔ］との比（α）＝［Ａ］／［Ｔ］を指標とする牛肉の熟成度の判定方法であり、（α）が０．１〜１．０、更には０．１〜０．５の範囲のとき熟成牛肉と判定するのが好ましい。（α）が０．１に満たないと熟成香りが少なく、熟成が足りない状態であり、１．０を越えると腐敗臭がわずかに認められるようになり熟成が度を超したことになるので、（α）は、この範囲にあることが好ましい。
また、熟成の経過と共に有意に増加が認められる牛肉の揮発性物質としては、ｎ−オクタナールの他に、ｎ−ヘプタン、トルエン、ヘキサン酸、トリメチルベンゼンの指標化合物がある。牛肉の揮発性物質を捕集した際に、これらの化合物の少なくとも一種を含む場合においても、これらの化合物の閾値［Ｔ］ｉと牛肉の揮発性物質を捕集した際の対応する化合物の濃度測定値［Ａ］ｉとの比（α）ｉが、好ましくは、０．０００００１〜０．０１、より好ましくは０．０００１〜０．００１の範囲にあり、ｎ−オクタナールの（α）が０．１〜１．０の範囲にあれば、より確実に熟成した牛肉と判定される。また、（α）ｉが０の場合とは、前記の選択された少なくとも一種の物質が検出されてはいるが（α）ｉが０．０００００１未満の場合を云い、そのとき、ｎ−オクタナールの（α）が０．１〜１．０の範囲にあればより確実に熟成した牛肉と判定される。
【００１１】
本発明においては、牛肉を４０℃以下で保存することが好ましい。前記の判定方法を熟成工程の工程管理手段として用い熟成度を判定し、熟成牛肉を製造することができる。すなわち、単に熟成経歴が未知の牛肉の熟成度を判定するのみでなく、販売状況の変化などにより熟成条件を変えて熟成させ、前記判定方法を用いて出荷時期を判断、調節したり、出荷時期に合わせた熟成条件（熟成温度の調整等）を採用するようにできる。一例を挙げれば、高温で保存し熟成させたり、或いは、低温で保存し熟成させたり、更に好ましくは、高温と低温とを組合わせて保存、熟成させるなど、目的に応じて温度条件を選ぶことができる。好ましい保存温度条件は、２０℃以下であり、更に好ましくは０〜５℃である。４０℃を超える温度では、牛肉が腐敗するおそれがある。なお、屠殺する牛の種類が一定であり、あるいは屠殺から出荷までの工程条件に変動が無いか小さい場合には、本発明の熟成度の判定方法を用いて予め熟成期間と熟成度の見極めをすることにより、熟成度判定の頻度を減らしたり、無くすことも可能である。
【００１２】
牛肉中のｎ−オクタナールの分析方法（ｎ−オクタナール濃度測定値の定量法）は、以下のように行った。ｎ−オクタナール以外の指定化合物であるヘキサン酸、ｎ−ヘプタン、トルエン、及びトリメチルベンゼンの濃度も同様にして分析する。
ミンチ状にした牛肉１０ｇおよびブロモベンセンなどの内部標準を浸み込ませた濾紙を１００ｍｌナス型フラスコに入れ、揮発性物質を８０℃で６０分間、吸着剤（ジーエルサイエンス社製、ＴｅｎａｘＧＲ）に吸着させ、濃縮導入装置付きＧＣ−ＭＳ（濃縮導入装置付きガスクロマトグラフィー・質量分析計）で分析し、得られた値を１０で除した測定値を牛肉１ｇ当たりのｎ−オクタナール濃度測定値（単位はｐｐｂ）とすることにより該化合物を定量することができる。
更に、以下のような方法でも牛肉中のｎ−オクタナールをはじめとした揮発性物質の測定をすることができる。
ミンチ状にした牛肉１ｇを１０ｍｌのバイアル（金属製のキャップとシリコン製の中栓を備えたガラス製容器）に入れ、５０℃で３０分間インキュベーションし、バイアル中の揮発性物質を５０００μｌシリンジにとり、複数の金属酸化物半導体センサー、例えば、スズ酸化物系のセンサーであるＳＹ／ＡＡ、Ｐ１０／１、ＰＡ２、Ｐ４０／１、Ｔ７０／２等に応答させ、得られた応答値の最大値を主成分分析等の統計解析を行い、別途ＧＣ−ＭＳを用いて検量した濃度と対応させることで、該化合物を定量（濃度測定値の単位はｐｐｂ）できる。
本発明の実施例では、濃縮導入装置付きＧＣ−ＭＳで該化合物の分析を行った。
【００１３】
【実施例】
以下、実施例により本発明を具体的に説明するが、本発明はこれらに限定されるものではない。
【００１４】
（実施例１）
屠殺後、すぐ０〜２℃で保存し、１日目を熟成１日目として、熟成６日（６日目）、熟成１０日（１０日目）、熟成完了（１４日目）にサンプリングした和牛ロース、約３００ｇをミンチ状にして１５ｇづつ小分けして、−４０℃で保存し、試験の度に解凍して分析した。ミンチ状にした各サンプル１０ｇおよび内部標準として５９．３２ｎｇ／μｌのブロムベンゼン−メタノール溶液を２μｌ浸み込ませた直径５ｍｍの円形の濾紙を１００ｍｌナス型フラスコに入れ、捕集セット（ジーエルサイエンス社製、銘柄：Ｔｅｎａｘ捕集セット）を用いて捕集揮発性物質を８０℃で６０分間、吸着剤（ジーエルサイエンス社製、銘柄：Ｔｅｎａｘ ＧＲ）に吸着させた。揮発性物質捕集後の吸着管（Ｔｅｎａｘ ＧＲ管）を濃縮試料導入装置（ＣＨＲＯＭＰＡＣＫ社製、Ｔｈｅｒｍａｌ ｄｅｓｏｒｐｔｉｏｎ ｃｏｌｄ ｔｒａｐ ｉｎｊｅｃｔｏｒ）付きのガスクロマトグラフ−質量分析計（ＧＣ−ＭＳ）（島津製作所製、ＱＰ−５０００）に装着し分析した。
本試験中のｎ−オクタナールの濃度測定値（単位はｐｐｂ）の経時変化を図１に示した。
以上の方法で有意差をもって経時的に増加している５つの物質を見つけることができた。これらの５種は、それぞれｎ−ヘプタン、トルエン、ヘキサン、ヘキサン酸、ｎ−オクタナール、トリメチルベンゼンであり、それらの濃度測定値（単位はｐｐｂ）の経時変化をにおい物質の量として図２に示した。更に、ＧＣ−ＭＳ分析で得られた結果（濃度測定値の単位はｐｐｂ）を、閾値（単位はｐｐｂ）で割ると、官能試験に則したデータ（図３では、におい指数と表示した。）となる。これを図３に示した。
【００１５】
（実施例２）
牛肉中のｎ−オクタナールの濃度測定値とｎ−オクタナールの閾値との比が０．３である牛肉について、下記の判定基準で５名による１回の官能検査を行った。ミンチ状にした牛肉１ｇを試験管に入れ、５℃で１時間放置後、官能試験を行った。なお、この試験に使用した牛肉は、４０℃以下の条件で保蔵されたものであった。
−１点：腐敗臭がする
０点：熟成香が少ない
１点：熟成香がする
２点：熟成香がよくする。
【００１６】
（比較例１）
牛肉中のｎ−オクタナールの濃度測定値とｎ−オクタナールの閾値との比が０．０５である牛肉について、上記の判定基準で５名による官能検査を行った。なお、この試験に使用した牛肉は、４０℃以下の条件で保蔵されたものであった。
【００１７】
（比較例２）
牛肉中のｎ−オクタナールの濃度測定値とｎ−オクタナールの閾値との比が１．２である牛肉について、上記の判定基準で５名による官能検査を行った。なお、この試験に使用した牛肉は、４０℃以下の条件で保蔵されたものであった。官能試験の結果を表１に示した。
【００１８】
【表１】
【発明の効果】
本発明によれば，牛肉の熟成度の判定を牛肉中のｎ−オクタナールの濃度を測定することにより行うことができ、正確且つ精度の高い熟成度の判定及びその判定方法を用いた熟成牛肉の製造方法を提供することが可能となった。
【図面の簡単な説明】
【図１】試料中のｎ−オクタナール量と貯蔵日数の関係を示すグラフ
【図２】試料中のｎ−ヘプタン、トルエン、ヘキサン酸、ｎ−オクタナール、トリメチルベンゼンのそれぞれの検出量と貯蔵日数の関係を示すグラフ
【図３】図２の５物質ｎ−ヘプタン、トルエン、ヘキサン酸、ｎ−オクタナール、トリメチルベンゼンをそれぞれの閾値で割った値と貯蔵日数の関係を示すグラフである。縦軸はにおい指数、即ちＧＣ−ＭＳで得られたデータを閾値で割った値である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for determining the degree of maturity of beef and a method for producing aged beef using the same. More specifically, the present invention relates to a method for judging the maturity of beef using n-octanal as an index when volatile substances of beef are collected, and a method for producing aged beef using the same.
[0002]
[Prior art]
In the food industry in recent years, three points of "deliciousness", "safety" and "simplicity" are keywords for product development. So far, research on food preservation has focused on "safety", which is the control of decay and the preservation of appearance, but with the increasing consumer demand for "deliciousness", improving "flavor". The necessity of research on methods began to be shouted. It has been recognized by consumers that some foods are stored under certain conditions, causing a phenomenon called ripening, and improving the flavor, which is an element of "deliciousness" such as taste and aroma.
It is known that beef, which has a strong demand for deliciousness, is stored under certain conditions, thereby causing aging, thereby improving the flavor, which is an element of "deliciousness" such as taste and aroma. However, ripening is a phenomenon that is likely to cause hygiene inconsistency, so making a mistake in one step will lead to putrefaction. Further, the judgment of the end of ripening depends on experience, and the judgment requires skilled skills and there is no objective standard at present.
[0003]
As means for judging the degree of ripening, for example, as described in Japanese Unexamined Patent Publication No. 6-50965, "Method of setting the shelf life of processed meat and judging method of aging", it is directly involved in the storage odor and peculiar aroma of processed meat. As a component to be used, 1,6-dioxacyclododecane-7,12-dione is used as an index to make it possible to set a best-before period and to judge the ripening degree. A method for determining the degree of maturity by measuring the aroma component increased by aging as in "Method of measuring beef maturity", and "Method of detecting beef maturation temperature history" in JP-A-6-261792. A method for detecting the aging temperature history using microorganisms is disclosed, but even if there is a clear indicator, the method for measurement is complicated, there is no clear indicator, Order or a constant is needed, it is difficult to carry out the determination of maturity.
[0004]
[Problems to be solved by the invention]
An object of the present invention is to provide a simple and highly accurate method for judging the maturity of beef, and to provide a method for producing delicious aged beef using the judgment method.
[0005]
[Means for Solving the Problems]
The present inventors have intensively studied the determination of the degree of maturity of beef in a simple and accurate manner. As a result, the collected beef volatile substances n-heptane, toluene, hexanoic acid, n-octanal, trimethylbenzene Increased over time, and found that n-octanal, which is an oxidation product of oleic acid, which is a major component of Wagyu beef lipid, was suitable as an indicator of maturation, and completed the present invention. .
[0006]
That is, the present invention provides the ratio (α) = [A] / [T] between the measured value [A] of the concentration of n-octanal and the threshold value [T] of n-octanal when the volatile substances of beef are collected. Provided is a method for determining the degree of maturity of beef as an index. In the above invention, there is provided a method for judging the degree of maturity of beef which is judged to be aged when (α) is in the range of 0.1 to 1.0. As an indicator compound when volatile substances of beef are collected, at least one compound selected from hexanoic acid excluding n-octanal, n-heptane, toluene, and trimethylbenzene is contained as an indicator compound, and the threshold value [T ] measured density values of the indicator compound and the corresponding i [a] ratio of i (α) i = [a ] i / [T] i is a method of determining the maturity of beef of the invention each 0 provide. It also contains at least one compound selected from hexanoic acid, n-heptane, toluene, and trimethylbenzene, and the threshold value [T] i of these compounds and the corresponding compounds when the volatile substances of beef are collected. concentration measurements [a] ratio of i (alpha) i provides a method for determining the maturity of beef of the invention in the range of 0.000001 to 0.01. Further, the present invention provides a method for producing an aged beef in which the beef is stored under a temperature condition of 40 ° C. or less and the shipping time is determined while judging the aging state using the beef aging degree judging method of the invention.
[0007]
BEST MODE FOR CARRYING OUT THE INVENTION
The type of beef applicable to the present invention is not particularly limited, and examples thereof include Wagyu, Holstein, and F1 obtained by multiplying Wagyu and Holstein. In a method for producing aged beef, usually, beef is slaughtered and processed for meat, and cooled at about 0 ° C. for about 14 days. At this stage, the beef is aged. Aged meat is shaped, packaged, stored and shipped for shipment. The aging of the beef was based on experience taking into account the time, taste and odor and the conditions of preservation through distribution to the consumer.
[0008]
The present inventors analyzed the volatile components of the beef samples for each aging process by using the bromobenzene-methanol solution as an internal standard and the analysis method shown in the Examples by a total ion gas chromatogram. 35 representative peaks were selected, analyzed for each peak area, and subjected to a significant difference test by a test for a difference between average values. Among 35 substances, it was found that n-heptane, toluene, hexanoic acid, n-octanal, and trimethylbenzene increased with time with a significant difference. In the present invention, these five compounds are referred to as indicator compounds of volatile substances of beef. The threshold values of these substances are 200,000 ppb for n-heptane, 50,000 ppb for toluene, 3000 ppb for hexanoic acid, 0.7 ppb for n-octanal, and 550 ppb for trimethylbenzene. As the threshold value in the present invention, the concentration of an aqueous solution (weight basis) is used for all of n-octanal, n-heptane, toluene, hexanoic acid, and trimethylbenzene. The threshold is the lowest concentration at which humans can detect its presence. The data implies that even the lowest concentration of n-octanal is felt in the human nose. In addition, the values (odor index) obtained by dividing the time-dependent changes of the five indicator compounds collected as volatile substances of beef by the respective threshold values are shown in FIG. 3, and this result shows that only n-octanal was used. Sensually.
Furthermore, n-octanal is a substance produced by biological reactions and rarely present in everyday living environments. Therefore, n-octanal is a substance suitable as an indicator compound for the measurement of maturity because it is different from a substance which exists in a normal environment such as heptane or toluene and is likely to be a pollutant (error source) for the measurement of maturity. It can be seen that it is.
[0009]
The present invention provides a method for judging the degree of maturity using n-octanal as an index of maturation of beef. The n-octanal is a colorless and transparent liquid having a boiling point of 171 to 173 ° C., which is called a straight-chain aldehyde having 8 carbon atoms, also called octylaldehyde or caprylaldehyde. The scent of n-octanal is oily or fruity, and is contained in orange and the like.
[0010]
According to the present invention, the ratio (α) between the measured value of the concentration of n-octanal [A] and the threshold value of n-octanal [T] (α) = [A] / [T] when the volatile matter of beef is collected is used as an index. It is a method of judging the degree of maturity of the beef, and when (α) is in the range of 0.1 to 1.0, more preferably 0.1 to 0.5, it is preferable to judge the beef as aged. If (α) is less than 0.1, the aging fragrance is low and aging is insufficient. If it exceeds 1.0, a rotten smell is slightly recognized and the aging has exceeded the degree. , (Α) are preferably in this range.
In addition to beef volatile substances that significantly increase with the aging process, besides n-octanal, there are indicator compounds such as n-heptane, toluene, hexanoic acid, and trimethylbenzene. Even if at least one of these compounds is contained when the volatile substances of beef are collected, the threshold value [T] i of these compounds and the concentration of the corresponding compound when the volatile substances of beef are collected The ratio (α) i to the measured value [A] i is preferably in the range of 0.000001 to 0.01, more preferably 0.0001 to 0.001, and (α) of n-octanal is 0. If it is in the range of 0.1 to 1.0, it is determined that the beef is more mature. The case where (α) i is 0 means that at least one kind of the selected substance is detected but (α) i is less than 0.000001. If (α) is in the range of 0.1 to 1.0, it is more reliably determined that the beef has matured.
[0011]
In the present invention, it is preferable to store beef at 40 ° C. or lower. By using the above-mentioned determination method as a process control means of the ripening step, the ripening degree is determined, and the ripened beef can be produced. That is, the aging history is not only to judge the maturity of the unknown beef, but also to change the aging conditions due to changes in the sales situation and the like, and to judge and adjust the shipping time using the above-mentioned determination method, and to adjust the shipping time. Aging conditions (adjustment of the aging temperature, etc.) can be adopted. One example is to store and ripen at a high temperature, or to store and ripen at a low temperature, and more preferably to store and ripen a combination of high and low temperature, and to select temperature conditions according to the purpose. Can be. Preferred storage temperature conditions are 20 ° C or lower, more preferably 0-5 ° C. If the temperature exceeds 40 ° C., beef may spoil. If the type of cattle to be slaughtered is constant, or if the process conditions from slaughter to shipping remain unchanged or small, the ripening period and the ripening degree are determined in advance using the ripening degree determination method of the present invention. By doing so, it is possible to reduce or eliminate the frequency of judging the maturity.
[0012]
The analysis method of n-octanal in beef (quantification method of measured value of n-octanal concentration) was performed as follows. The concentrations of the specified compounds other than n-octanal, hexanoic acid, n-heptane, toluene, and trimethylbenzene, are analyzed in the same manner.
A filter paper impregnated with 10 g of minced beef and an internal standard such as bromobenzene is placed in a 100 ml eggplant-shaped flask, and volatile substances are adsorbed to an adsorbent (Tenax GR, manufactured by GL Sciences Inc.) at 80 ° C. for 60 minutes. And analyzed by a GC-MS equipped with a concentration introducing device (gas chromatography / mass spectrometer equipped with a concentration introducing device), and a measured value obtained by dividing the obtained value by 10 is a measured value of n-octanal concentration per 1 g of beef (unit). Ppb), the compound can be quantified.
Further, volatile substances such as n-octanal in beef can be measured by the following method.
1 g of minced beef is placed in a 10 ml vial (glass container having a metal cap and a silicon inner plug), incubated at 50 ° C. for 30 minutes, and a volatile substance in the vial is taken up with a 5000 μl syringe, A plurality of metal oxide semiconductor sensors, for example, tin oxide based sensors SY / AA, P10 / 1, PA2, P40 / 1, T70 / 2, etc., are responded, and the maximum value of the obtained response value is mainly determined. The compound can be quantified (the unit of the measured concentration value is ppb) by performing statistical analysis such as component analysis and making it correspond to the concentration separately calibrated using GC-MS.
In Examples of the present invention, the compound was analyzed by GC-MS with a concentration introducing device.
[0013]
【Example】
Hereinafter, the present invention will be described specifically with reference to Examples, but the present invention is not limited thereto.
[0014]
(Example 1)
Immediately after sacrifice, it was stored immediately at 0 to 2 ° C., and sampled at 6 days (6 days), 10 days (10 days), and maturation completed (14 days), with the first day as the first day of ripening. Approximately 300 g of Japanese beef loin was minced, divided into 15 g portions, stored at −40 ° C., thawed at each test, and analyzed. 10 g of each minced sample and a 5 mm-diameter circular filter paper impregnated with 2 μl of a bromobenzene-methanol solution of 59.32 ng / μl as an internal standard were put in a 100 ml eggplant-shaped flask, and a collection set (GL Science Co., Ltd.) And brand name: Tenax collection set), and the collected volatile substances were adsorbed to an adsorbent (brand name: Tenax GR) at 80 ° C. for 60 minutes. A gas chromatograph-mass spectrometer (GC-MS) equipped with a concentrated sample introduction device (manufactured by CHROMPACK, Thermal desorption cold trap injector) (GC-MS) (manufactured by Shimadzu Corporation, QP- 5000) and analyzed.
FIG. 1 shows the change over time in the measured value of n-octanal (unit: ppb) during the test.
With the above method, five substances which increased with time with a significant difference could be found. These five types are n-heptane, toluene, hexane, hexanoic acid, n-octanal, and trimethylbenzene, respectively, and the change over time in the measured concentration (unit: ppb) is shown in FIG. Was. Furthermore, when the result obtained by the GC-MS analysis (the unit of the measured concentration value is ppb) is divided by a threshold value (the unit is ppb), data conforming to a sensory test (in FIG. 3, indicated as an odor index). It becomes. This is shown in FIG.
[0015]
(Example 2)
For beef in which the ratio of the measured value of n-octanal in beef to the threshold value of n-octanal was 0.3, one sensory test was conducted by five persons according to the following criteria. 1 g of minced beef was placed in a test tube, and left at 5 ° C. for 1 hour, and then subjected to a sensory test. The beef used in this test was stored under conditions of 40 ° C. or lower.
-1 point:
[0016]
(Comparative Example 1)
For beef in which the ratio of the measured value of the concentration of n-octanal in the beef to the threshold value of n-octanal was 0.05, a sensory test was conducted by five persons according to the above-mentioned criteria. The beef used in this test was stored under conditions of 40 ° C. or lower.
[0017]
(Comparative Example 2)
For beef in which the ratio of the measured value of n-octanal in beef to the threshold value of n-octanal was 1.2, a sensory test was conducted by five persons according to the above-mentioned criteria. The beef used in this test was stored under conditions of 40 ° C. or lower. Table 1 shows the results of the sensory test.
[0018]
[Table 1]
【The invention's effect】
According to the present invention, the determination of the degree of maturity of the beef can be performed by measuring the concentration of n-octanal in the beef. It has become possible to provide a manufacturing method.
[Brief description of the drawings]
FIG. 1 is a graph showing the relationship between the amount of n-octanal in a sample and the number of storage days. FIG. 2 is a graph showing the respective detected amounts and storage days of n-heptane, toluene, hexanoic acid, n-octanal, and trimethylbenzene in the sample. FIG. 3 is a graph showing the relationship between values obtained by dividing the five substances n-heptane, toluene, hexanoic acid, n-octanal, and trimethylbenzene in FIG. 2 by respective threshold values and the number of storage days. The vertical axis is an odor index, that is, a value obtained by dividing data obtained by GC-MS by a threshold value.
Claims (5)
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| JP2002179229A JP2004020499A (en) | 2002-06-19 | 2002-06-19 | Method of determining maturation degree of beef, and method of manufacturing mature beef using the same |
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| JP2002179229A JP2004020499A (en) | 2002-06-19 | 2002-06-19 | Method of determining maturation degree of beef, and method of manufacturing mature beef using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101156093B1 (en) | 2010-07-23 | 2012-06-20 | 충남대학교산학협력단 | Method for breed detection of meat using volatile compounds profile |
| JP2013231711A (en) * | 2012-04-02 | 2013-11-14 | Hitachi High-Technologies Corp | Method of analyzing volatile substance included in sample liquid |
| CN106501471A (en) * | 2016-11-02 | 2017-03-15 | 济南趵突泉酿酒有限责任公司 | A kind of method of prediction low alcohol white spirit shelf life |
| JP2018141741A (en) * | 2017-02-28 | 2018-09-13 | 高砂香料工業株式会社 | Method of evaluating contribution of perfume compounds in retronasal aroma |
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2002
- 2002-06-19 JP JP2002179229A patent/JP2004020499A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101156093B1 (en) | 2010-07-23 | 2012-06-20 | 충남대학교산학협력단 | Method for breed detection of meat using volatile compounds profile |
| JP2013231711A (en) * | 2012-04-02 | 2013-11-14 | Hitachi High-Technologies Corp | Method of analyzing volatile substance included in sample liquid |
| CN106501471A (en) * | 2016-11-02 | 2017-03-15 | 济南趵突泉酿酒有限责任公司 | A kind of method of prediction low alcohol white spirit shelf life |
| JP2018141741A (en) * | 2017-02-28 | 2018-09-13 | 高砂香料工業株式会社 | Method of evaluating contribution of perfume compounds in retronasal aroma |
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