WO2013125612A1 - Simple method for measuring median particle size of lactic food - Google Patents

Simple method for measuring median particle size of lactic food Download PDF

Info

Publication number
WO2013125612A1
WO2013125612A1 PCT/JP2013/054260 JP2013054260W WO2013125612A1 WO 2013125612 A1 WO2013125612 A1 WO 2013125612A1 JP 2013054260 W JP2013054260 W JP 2013054260W WO 2013125612 A1 WO2013125612 A1 WO 2013125612A1
Authority
WO
WIPO (PCT)
Prior art keywords
particle size
milk
absorbance
correlation
dairy
Prior art date
Application number
PCT/JP2013/054260
Other languages
French (fr)
Japanese (ja)
Inventor
阪田　匡
芙由子 山本
Original Assignee
株式会社明治
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社明治 filed Critical 株式会社明治
Priority to JP2014500750A priority Critical patent/JP6196610B2/en
Priority to CN201380010383.4A priority patent/CN104136906A/en
Publication of WO2013125612A1 publication Critical patent/WO2013125612A1/en

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0042—Investigating dispersion of solids
    • G01N2015/0053—Investigating dispersion of solids in liquids, e.g. trouble
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N2015/0277—Average size only
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G01N21/53—Scattering, i.e. diffuse reflection within a body or fluid within a flowing fluid, e.g. smoke
    • G01N21/534—Scattering, i.e. diffuse reflection within a body or fluid within a flowing fluid, e.g. smoke by measuring transmission alone, i.e. determining opacity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02—Food
    • G01N33/04—Dairy products

Definitions

  • the present invention relates to a simple method for measuring the 50% particle size of dairy foods. Specifically, the present invention relates to a simple method for measuring the 50% particle size of dairy foods, which uses a measured value of absorbance by light irradiation at a specific wavelength.
  • the stalactic food particles are composed of fat globules and protein particles (such as casein micelles), and their dimensions are controlled by homogenization treatment or emulsification treatment.
  • fat globules and protein particles such as casein micelles
  • emulsification treatment for example, as a typical dairy food, since milk has a large fat globule size during milking, the fat globule tends to float as it is, and so-called creaming (fat flotation) phenomenon is observed. For this reason, creaming is suppressed by homogenizing using a homogenizer (homogenizer), reducing the size of fat globules, and delaying the rising speed of fat globules (Non-patent Document 1).
  • homogenizer homogenizer
  • fat globules diameter affects the flavor and texture. That is, it is a known fact that in milk foods, even if the nutritional composition (lipid, protein, sugar, ash, etc.) is the same, if the fat globule diameter is different, the flavor and texture change. By increasing the value, the richness can be enhanced.
  • dairy food particles affect the flavor and texture.
  • the dairy food is used as a dispersion, the average value of the volume-based particle size distribution measurement results is “50% particle size”.
  • a typical apparatus for measuring the “50% particle size” of this milky food is a laser diffraction type particle size distribution measuring apparatus (manufactured by Shimadzu Corporation) (Patent Documents 1 to 4). Therefore, if such a particle size distribution measuring device can be introduced, the 50% particle size of dairy foods can be reliably measured, but it can always be easily introduced in consideration of actual purchase costs, maintenance costs, repair costs, etc. It's hard to say.
  • a method of estimating the 50% particle size of dairy foods has been adopted from past experience after considering the shearing effect in homogenization processing of dairy foods. It was. For example, in order to suppress the creaming of milk, homogenization was performed at a high pressure of a predetermined value or more to reduce the size of fat globules. At this time, the 50% particle size of actual milk is measured each time. It never happened.
  • the present inventors have conducted extensive research and have obtained the following knowledge. That is, it is found that there is a correlation between the measured value of absorbance by light irradiation of a specific wavelength and the measured value of 50% particle size of dairy food by a particle size distribution measuring device, and by using this, particle size distribution measurement is performed. It has been found that the 50% particle size of dairy food can be measured easily and inexpensively without introducing a large and expensive equipment such as an apparatus, and the present invention has been completed.
  • the present invention is as follows.
  • [1] A simple method for measuring the 50% particle size of dairy foods, which uses a correlation between a measured value of absorbance by light irradiation and a measured value of 50% particle size by a particle size distribution measuring device.
  • [2] The simple method for measuring 50% particle size of a dairy food according to the above [1], wherein the correlation is a proportional relationship.
  • [3] The simple method for measuring a 50% particle size of a dairy food according to the above [1] or [2], wherein the light irradiation has a wavelength of 500 nm to 1100 nm.
  • [4] The simple method for measuring a 50% particle size of a dairy food according to any one of the above [1] to [3], wherein the light irradiation has a wavelength of 800 nm to 1100 nm.
  • [5] Simple measurement of 50% particle size of dairy food according to any one of [1] to [4] above, wherein the 50% particle size of the dairy food is 0.1 to 2.0 ⁇ m Method.
  • [6] The above-mentioned [1], wherein the dairy food is animal milk, processed animal milk, animal milk drink, soft drink with animal milk, plant milk, processed vegetable milk, vegetable milk drink, or soft drink with vegetable milk.
  • the present invention it is found that there is a correlation between the 50% particle size of dairy foods and the measurement value of absorbance by light irradiation, and there are few restrictions on locations and devices, and stable absorbance can be obtained. Therefore, it is possible to provide a simple and inexpensive method for measuring the 50% particle size of dairy foods without using a large and special equipment such as a particle size distribution measuring apparatus. And in this invention, since the 50% particle diameter of dairy foods can be simply measured using a highly versatile spectrophotometer, the quality (flavor, texture, physical properties, etc.) of dairy foods is easy. Can provide management, control and design methods.
  • the present invention relates to a simple method for measuring the 50% particle size of dairy foods, which uses a measured value of absorbance by light irradiation.
  • the absorbance measurement value by light irradiation is not particularly limited as long as it can be measured using a known principle.
  • a spectrophotometer because the absorbance due to light irradiation can be measured easily and inexpensively and is highly versatile.
  • the spectrophotometer is not particularly limited as long as it is a known specification. However, since it can measure the difference in absorbance between the measurement sample and the control sample, the double beam type is preferable, and the spectrophotometer UV-1600PC (manufactured by Shimadzu Corporation) is preferable. ) And the like. Once installed, this spectrophotometer can be used stably for a long time.
  • the absorbance measurement temperature is not particularly limited as long as the measurement sample or the target sample is liquid, but specifically, 10 ° C. to 30 ° C. is preferable from the viewpoint of ease of handling of the measurement sample and the target sample. 15 to 30 ° C. is more preferable, and 20 to 25 ° C. is more preferable.
  • the wavelength of light irradiation is not particularly limited as long as the correlation with the 50% particle size of the dairy food can be expressed by a regression curve, a regression line, or the like.
  • the light irradiation since the correlation between the absorbance by light irradiation and the 50% particle size of the dairy food is clear, it is preferable that the light irradiation has a wavelength of 500 nm to 1100 nm (near infrared region), More preferably, the light irradiation has a wavelength of 800 nm to 1100 nm.
  • the 50% particle size of the dairy food is 0 because the correlation between the measured value of the absorbance by light irradiation and the measured value of the 50% particle size of the dairy food by the particle size distribution measuring device is clear. It is preferably 1 to 2.5 ⁇ m, more preferably 0.2 to 2.0 ⁇ m, further preferably 0.3 to 2.0 ⁇ m, and 0.4 to 2.0 ⁇ m. Is particularly preferred. If the 50% particle size of the dairy food is larger than 2.5 ⁇ m, it is easy to deviate from the correlation of the calibration curve. Hard to do.
  • the 50% particle diameter measured value by the particle size distribution measuring device is not particularly limited as long as it can be measured using a known principle. At this time, in the present invention, it is preferable to use a particle size distribution measuring device because the 50% particle size can be measured easily and inexpensively and has high versatility.
  • the measured value of the 50% particle size by the particle size distribution measuring device is 50% of the integrated value with respect to the result of measuring the particle size distribution of the dispersion such as dairy food by the laser diffraction / scattering method.
  • the particle size of 50% in terms of the integrated value is the particle size when the number of particles is added from the smaller particle size and reaches 50% of the total number of particles.
  • the measured value of 50% particle diameter is sometimes referred to as average fat globule diameter.
  • 50% particle diameter includes the meaning of average fat globule diameter. Is done.
  • dairy foods are milk-containing (liquid) foods, milk-derived raw materials, processed products thereof, and the like, and are not particularly limited.
  • animal milk derived from cows, sheep, goats, buffalos, processed animal milk, animal milk drinks, soft drinks containing animal milk, plant milk derived from soybeans, processed vegetable milk, vegetable milk drinks Since it is preferably a soft drink containing vegetable milk and is typically distributed in the market, it is more preferable that animal milk is cow milk and plant milk is soy milk.
  • artificial milk constituted by emulsifying vegetable oil and other raw materials is also included in the vegetable milk.
  • the dairy food is not particularly limited, for example, to the degree of milk reduction or processing.
  • concentrated whole milk, whole milk powder, partially skimmed milk, partially skimmed concentrated milk, partially skimmed milk powder, skimmed milk, skimmed concentrated milk, skimmed milk powder, cream in addition to raw milk and milk sterilized raw milk, concentrated whole milk, whole milk powder, partially skimmed milk, partially skimmed concentrated milk, partially skimmed milk powder, skimmed milk, skimmed concentrated milk, skimmed milk powder, cream,
  • the present invention can also be applied to reduced dairy products such as butter by reducing them to liquid form.
  • processed milk prepared by mixing milk and dairy products to the required composition processed milk obtained by membrane treatment of milk to concentrate and remove various ingredients, milk drinks including milk, dairy products and processed milk
  • the present invention can also be applied to soft drinks containing milk. And these can apply this invention similarly to animal milk and vegetable milk other than milk.
  • the dairy food can be arbitrarily added with foods other than animal milk or vegetable milk, various food additives, etc., in accordance with product characteristics.
  • food includes salmon, tea, fruit juice, sugar, high-intensity sweetener, and the like
  • food additives include stabilizers, thickeners, preservatives, minerals such as calcium, and flavors. Etc.
  • the present invention has found that there is a correlation between the 50% particle size of dairy foods and the absorbance measured by light irradiation. That is, obtaining a 50% particle size of at least two dairy foods using a conventional particle size distribution measuring device, obtaining an absorbance of the dairy food by light irradiation, and correlation between the 50% particle size and the absorbance. A step of determining the relationship, and a simple measurement method of 50% particle size of an unknown milk food using the correlation. “Correlation” as used herein means that, for example, a function (primary, secondary, etc.) relationship is established between the absorbance and the 50% particle size. Due to the correlation, an unknown 50% particle size can be easily measured by absorbance.
  • a specific method of determining is to select at least two samples as sampling, measure the 50% particle diameter using the particle size distribution measuring apparatus as described above, and obtain a sample having a 50% particle diameter.
  • the 50% particle size of the dairy food is determined by, for example, nonlinear least square method or linearity with respect to the correlation between the measured value of absorbance by light irradiation and the measured value of 50% particle size by a particle size distribution measuring device.
  • a known approximation method such as a least square method is applied.
  • the correlation can be calculated in advance using a mathematical formula or the like, and the absorbance of the measurement sample or the control sample can be actually measured and applied to the correlation mathematical formula or the like.
  • the 50% particle size of the dairy food is not particularly limited as long as it is calculated using the correlation between the measured value of absorbance by light irradiation and the measured value of 50% particle size by a particle size distribution measuring device.
  • the correlation between the measured value of absorbance at which light irradiation is at a wavelength of 500 nm to 1100 nm and the measured value of 50% particle size by a particle size distribution measuring device is calculated using a calibration curve or a scientific calculator, and then linear The least square method is applied, and mathematical formulas and conversion coefficients are calculated in advance. Then, the absorbance of the measurement sample and the control sample is actually measured, and the 50% particle size of the dairy food is calculated by applying the mathematical formula and the conversion factor calculated in advance.
  • the correlation coefficient (R 2 ) of the linear least square method such as a calibration curve is preferably 0.90 or more, more preferably 0.93 or more, and further preferably 0.95 or more. If the correlation coefficient of the linear least squares method is less than 0.90, the accuracy of the calibration curve is lowered, and there is a possibility that the 50% particle diameter of dairy foods cannot be accurately calculated.
  • the spectrophotometer UV-1600PC (manufactured by Shimadzu Corporation) is exemplified as the absorbance measuring apparatus
  • the laser diffraction particle size distribution measuring apparatus SALD-2001 system (manufactured by Shimadzu Corporation) is exemplified as the particle size distribution measuring apparatus.
  • these devices may not necessarily exist due to renewal or version upgrade of these devices.
  • the present invention can be implemented regardless of the manufacturer, model, model number, etc., as long as it is an alternative device having the same function that is actually distributed or sold.
  • the measured value of absorbance by light irradiation and the measured value of 50% particle size by the particle size distribution measuring device are measured by these alternative devices, and the correlation between the measured values is used to determine 50% of milk food. Needless to say, the particle size can be calculated.
  • Test Example 1 Prepare raw milk (non-fat milk solid content: 8.7%, milk fat content: 4.1%) at 3kg, heat from 10 ° C to 60 ° C while stirring in a small stainless steel container, Using a homogenizer (NS1001, manufactured by Niro Soavi), homogenization treatment was performed at five pressures shown in Table 1. After dispensing these 5 types of unheated milk in a heat-resistant container, using an autoclave, heating at 110 ° C. for 1 minute, cooling to 10 ° C. or less with ice water, and then 5 types of heated milk (milk) Were prepared (Samples 1 to 5).
  • the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm.
  • Absorbance at 1100 nm was measured, and a 50% particle size was measured using a particle size distribution analyzer (SALD-2001, manufactured by Shimadzu Corporation). The results are shown in Table 1. Further, the correlation between the absorbance at each wavelength and the 50% particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 2.
  • Test Example 2 40 g of heated milk prepared in Test Example 1 (Sample 1), 16 g of a commercially available sugar-free koji beverage (“Seven Premium Unsweetened Coffee”), 5.6 g of sugar, and 18.4 g of raw water are prepared. And mixed each. This mixture was dispensed into a heat-resistant container and then heated at 110 ° C. for 1 minute using an autoclave, and then cooled to 10 ° C. or lower with ice water to prepare a milk drink (Sample 6). In the same manner as described above, milk drinks were also prepared for the heated milk prepared in Example 1 (Samples 2 to 5) (Samples 7 to 10).
  • the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation). Absorbance at 1100 nm was measured, and a 50% particle size was measured using a particle size distribution meter (SALD-2001, manufactured by Shimadzu Corporation). The results are shown in Table 3. Further, the correlation between the absorbance at each wavelength and the 50% particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 4.
  • the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation).
  • UV-1600PC UV-1600PC
  • SALD-2001 particle size distribution meter
  • the correlation between the absorbance and the 50% particle size was not proportional and could not be approximated linearly. That is, it was found that the correlation between absorbance and 50% particle diameter was confirmed in heated milk (milk) and also in processed milk prepared from reduced milk raw materials.
  • Test Example 4 52680 g of raw milk, 2070 g of nonfat concentrated milk, and 5250 g of raw water were prepared and mixed. This mixed milk (non-fat milk solid content: 8.8%, milk fat content: 3.6%) was heated from 10 ° C. to 60 ° C. with stirring in a tank, and then used with a homogenizer (homogenizer). Homogenization was performed at three types of pressure shown in Table 7. These three types of unheated processed milk are preheated at 85 ° C. using a plate heat exchanger, heated at 130 ° C. for 2 seconds, cooled to 10 ° C. or lower, and then heated to three types of heated processed milk ( Processed milk) (samples 16-18).
  • the present invention it is found that there is a correlation between the 50% particle size of dairy foods and the measurement value of absorbance by light irradiation, and there are few restrictions on locations and devices, and stable absorbance can be obtained. Therefore, it is possible to provide a simple and inexpensive method for measuring the 50% particle size of dairy foods without using a large and special equipment such as a particle size distribution measuring apparatus. And in this invention, since the 50% particle diameter of dairy foods can be simply measured using a highly versatile spectrophotometer, the quality (flavor, texture, physical properties, etc.) of dairy foods is easy. Can provide management, control and design methods.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Dairy Products (AREA)

Abstract

[Problem] To provide a method for easily and economically measuring the median particle size of a lactic food without using a large-scale special apparatus such as a particle size distribution measuring device. [Solution] By finding that there is an almost linear function correlation between measured values of absorbance at light irradiation of a specific wavelength and the median particle size of a lactic food and forming a calibration curve that serves as an indication of the correlation, etc., the median particle size of a lactic food is easily and economically measured using a spectrophotometer which can be more easily installed than a particle size distribution measuring device.

Description

乳性食品の５０％粒子径の簡易測定方法Simple measurement method for 50% particle size of dairy foods
  本発明は、乳性食品の５０％粒子径の簡易測定方法に関する。具体的には、特定の波長の光照射による吸光度の測定値を利用する、乳性食品の５０％粒子径の簡易測定方法に関する。 The present invention relates to a simple method for measuring the 50% particle size of dairy foods. Specifically, the present invention relates to a simple method for measuring the 50% particle size of dairy foods, which uses a measured value of absorbance by light irradiation at a specific wavelength.
  乳性食品の粒子は、脂肪球やタンパク質粒子（カゼインミセルなど）で構成されており、均質化処理や乳化処理などにより、その寸法が制御される。例えば乳性食品の代表的なものとして、牛乳では搾乳時に、脂肪球の寸法が大きいため、そのままでは、脂肪球が浮上しやすく、いわゆるクリーミング（脂肪浮上）の現象が見られる。そのため、均質機（ホモゲナイザー）を用いて均質化処理し、脂肪球の寸法を小さくして、脂肪球の浮上速度を遅らせることで、クリーミングを抑制している（非特許文献１）。 The stalactic food particles are composed of fat globules and protein particles (such as casein micelles), and their dimensions are controlled by homogenization treatment or emulsification treatment. For example, as a typical dairy food, since milk has a large fat globule size during milking, the fat globule tends to float as it is, and so-called creaming (fat flotation) phenomenon is observed. For this reason, creaming is suppressed by homogenizing using a homogenizer (homogenizer), reducing the size of fat globules, and delaying the rising speed of fat globules (Non-patent Document 1).
  また、乳性食品では、脂肪球の寸法、いわゆる脂肪球径が風味や食感に影響することが知られている。すなわち、乳性食品では、栄養組成（脂質、タンパク質、糖質、灰分など）が同じでも、脂肪球径が異なると、風味や食感などが変わることは既知の事実であり、例えば脂肪球径を大きくすることで、濃厚感を高められることになる。 In addition, in milky foods, it is known that the size of fat globules, the so-called fat globules diameter, affects the flavor and texture. That is, it is a known fact that in milk foods, even if the nutritional composition (lipid, protein, sugar, ash, etc.) is the same, if the fat globule diameter is different, the flavor and texture change. By increasing the value, the richness can be enhanced.
  上記の通り、乳性食品の粒子は、風味や食感に影響するが、このとき、乳性食品を分散体とすると、体積基準の粒度分布の測定結果の平均値を「５０％粒子径」として代用することが多い。そして、この乳性食品の「５０％粒子径」を測定する代表的な機器には、レーザー回折式の粒度分布測定装置（島津製作所製）などがある（特許文献１～４）。そこで、このような粒度分布測定装置を導入できれば、乳性食品の５０％粒子径を確実に測定できることとなるが、実際の購入費や維持費・修繕費などを勘案すると、必ずしも手軽に導入できるとは言い難い。 As described above, dairy food particles affect the flavor and texture. At this time, when the dairy food is used as a dispersion, the average value of the volume-based particle size distribution measurement results is “50% particle size”. Often used as a substitute. A typical apparatus for measuring the “50% particle size” of this milky food is a laser diffraction type particle size distribution measuring apparatus (manufactured by Shimadzu Corporation) (Patent Documents 1 to 4). Therefore, if such a particle size distribution measuring device can be introduced, the 50% particle size of dairy foods can be reliably measured, but it can always be easily introduced in consideration of actual purchase costs, maintenance costs, repair costs, etc. It's hard to say.
  従って、粒度分布測定装置を導入していない場合、乳性食品の均質化処理における剪断効果を考慮した上で、過去の経験から、乳性食品の５０％粒子径を推測する方法などを採用してきた。例えば牛乳のクリーミングを抑制するためには、所定値以上の高圧で均質化処理し、脂肪球の寸法を小さくしてきたが、このとき、その都度では、実際の牛乳の５０％粒子径を測定することはなかった。 Therefore, when a particle size distribution measuring device is not introduced, a method of estimating the 50% particle size of dairy foods has been adopted from past experience after considering the shearing effect in homogenization processing of dairy foods. It was. For example, in order to suppress the creaming of milk, homogenization was performed at a high pressure of a predetermined value or more to reduce the size of fat globules. At this time, the 50% particle size of actual milk is measured each time. It never happened.
特開平１１－００９１８７JP-A-11-009187 特開２００１－２９２７１６JP 2001-292716 A 特開２００４－２６７１５３JP 2004-267153 A ＷＯ２００２／０３７９８５WO2002 / 037985
  このような状況に鑑み、本発明では、粒度分布測定装置のような大掛かりで特殊な設備を使用せずに、乳性食品（液状乳性食品の脂肪球径やタンパク質粒子径など）の５０％粒子径を簡便で安価に測定する方法を提供することを課題とする。 In view of such circumstances, in the present invention, 50% of dairy foods (such as fat sphere diameter and protein particle diameter of liquid dairy foods) are used without using large and special equipment such as a particle size distribution measuring device. It is an object of the present invention to provide a simple and inexpensive method for measuring the particle size.
  本発明者らは、上記の課題に鑑み、鋭意研究を進めたところ、以下の知見を得た。すなわち、特定の波長の光照射による吸光度の測定値と粒度分布測定装置による乳性食品の５０％粒子径の測定値とに相関関係があることを見出し、これを利用することで、粒度分布測定装置のような大掛かりで高価な設備を導入しなくとも、乳性食品の５０％粒子径を簡便で安価に測定できることを見出し、本発明を完成するに至った。 In light of the above problems, the present inventors have conducted extensive research and have obtained the following knowledge. That is, it is found that there is a correlation between the measured value of absorbance by light irradiation of a specific wavelength and the measured value of 50% particle size of dairy food by a particle size distribution measuring device, and by using this, particle size distribution measurement is performed. It has been found that the 50% particle size of dairy food can be measured easily and inexpensively without introducing a large and expensive equipment such as an apparatus, and the present invention has been completed.
  具体的には、５００ｎｍ～１１００ｎｍの波長の光照射による吸光度の測定値と粒度分布測定装置による乳性食品の５０％粒子径の測定値とに一次関数的な相関関係（比例関係）があることを見出し、この相関関係の指標となる検量線を予め作成などすることで、粒度分布測定装置よりも簡易的に設置できる分光光度計を使用して、乳性食品の５０％粒子径を簡便で安価に測定できることを見出した。 Specifically, there is a linear function correlation (proportional relationship) between the measured value of absorbance by light irradiation with a wavelength of 500 nm to 1100 nm and the measured value of 50% particle size of milk food by a particle size distribution measuring device. By using a spectrophotometer that can be installed more simply than a particle size distribution measuring device by preparing a calibration curve that is an index of this correlation in advance, the 50% particle size of dairy foods can be simplified. We found that it can be measured at low cost.
  すなわち、本発明は、次の通りとなる。
  ［１］  光照射による吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値との相関関係を利用することを特徴とする乳性食品の５０％粒子径の簡易測定方法。
  ［２］  相関関係が比例関係であることを特徴とする前記［１］記載の乳性食品の５０％粒子径の簡易測定方法。
　［３］  光照射が５００ｎｍ～１１００ｎｍの波長であることを特徴とする前記［１］又は［２］記載の乳性食品の５０％粒子径の簡易測定方法。
  ［４］  光照射が８００ｎｍ～１１００ｎｍの波長であることを特徴とする前記［１］～［３］の何れか記載の乳性食品の５０％粒子径の簡易測定方法。
  ［５］  乳性食品の５０％粒子径が０．１～２．０μｍであることを特徴とする前記［１］～［４］の何れか記載の乳性食品の５０％粒子径の簡易測定方法。
  ［６］  乳性食品が獣乳、加工獣乳、獣乳飲料、獣乳入り清涼飲料、植物乳、加工植物乳、植物乳飲料、植物乳入り清涼飲料であることを特徴とする前記［１］～［５］の何れか記載の乳性食品の５０％粒子径の簡易測定方法。
  ［７］  獣乳が牛乳であり、植物乳が豆乳であることを特徴とする前記［６］記載の乳性食品の５０％粒子径の簡易測定方法。
  ［８］  吸光度を分光光度計で測定することを特徴とする前記［１］～［７］の何れか記載の乳性食品の５０％粒子径の簡易測定方法。 That is, the present invention is as follows.
[1] A simple method for measuring the 50% particle size of dairy foods, which uses a correlation between a measured value of absorbance by light irradiation and a measured value of 50% particle size by a particle size distribution measuring device.
[2] The simple method for measuring 50% particle size of a dairy food according to the above [1], wherein the correlation is a proportional relationship.
[3] The simple method for measuring a 50% particle size of a dairy food according to the above [1] or [2], wherein the light irradiation has a wavelength of 500 nm to 1100 nm.
[4] The simple method for measuring a 50% particle size of a dairy food according to any one of the above [1] to [3], wherein the light irradiation has a wavelength of 800 nm to 1100 nm.
[5] Simple measurement of 50% particle size of dairy food according to any one of [1] to [4] above, wherein the 50% particle size of the dairy food is 0.1 to 2.0 μm Method.
[6] The above-mentioned [1], wherein the dairy food is animal milk, processed animal milk, animal milk drink, soft drink with animal milk, plant milk, processed vegetable milk, vegetable milk drink, or soft drink with vegetable milk. ] A simple method for measuring the 50% particle size of a dairy food according to any one of [5] to [5].
[7] The simple method for measuring a 50% particle size of a dairy food according to the above [6], wherein the animal milk is cow milk and the plant milk is soy milk.
[8] The simple method for measuring 50% particle size of a dairy food according to any one of [1] to [7], wherein the absorbance is measured with a spectrophotometer.
  本発明では、乳性食品の５０％粒子径と、光照射による吸光度の測定値との間に相関関係が存在していることを見出し、ロケーションや装置の制限が少なく、安定した吸光度が得られることから、粒度分布測定装置のような大掛かりで特殊な設備を使用せずに、乳性食品の５０％粒子径を簡便で安価に測定する方法を提供できる。そして、本発明では、汎用性の高い分光光度計を使用して、乳性食品の５０％粒子径を簡易的に測定できるため、乳性食品の品質（風味、食感、物性など）を容易に管理・制御・設計などする方法を提供できる。 In the present invention, it is found that there is a correlation between the 50% particle size of dairy foods and the measurement value of absorbance by light irradiation, and there are few restrictions on locations and devices, and stable absorbance can be obtained. Therefore, it is possible to provide a simple and inexpensive method for measuring the 50% particle size of dairy foods without using a large and special equipment such as a particle size distribution measuring apparatus. And in this invention, since the 50% particle diameter of dairy foods can be simply measured using a highly versatile spectrophotometer, the quality (flavor, texture, physical properties, etc.) of dairy foods is easy. Can provide management, control and design methods.
  以下では、本発明を詳細に説明するが、本発明は、個々の形態には限定されない。 In the following, the present invention will be described in detail, but the present invention is not limited to individual forms.
  本発明は、光照射による吸光度の測定値を利用することを特徴とする乳性食品の５０％粒子径の簡易測定方法に関するものである。 The present invention relates to a simple method for measuring the 50% particle size of dairy foods, which uses a measured value of absorbance by light irradiation.
  本発明において、光照射による吸光度の測定値は、公知の原理を用いて測定できれば、特に限定されない。このとき、本発明では、光照射による吸光度を簡便で安価に測定でき、汎用性も高いため、分光光度計を使用することが好ましい。なお、この分光光度計は、公知の仕様であれば、特に限定されないが、測定試料と対照試料との吸光度差を測定できるため、ダブルビーム式が好ましく、分光光度計ＵＶ－１６００ＰＣ（島津製作所製）などを例示できる。この分光光度計は、いったん導入して設置すれば長期的に安定して使用できる。また、吸光度の測定温度は、測定試料や対象試料などが液状であれば、特に限定されないが、具体的には、測定試料や対象試料の取扱いの容易さなどから、１０℃～３０℃が好ましく、１５℃～３０℃がより好ましく、２０℃～２５℃がさらに好ましい。 In the present invention, the absorbance measurement value by light irradiation is not particularly limited as long as it can be measured using a known principle. At this time, in the present invention, it is preferable to use a spectrophotometer because the absorbance due to light irradiation can be measured easily and inexpensively and is highly versatile. The spectrophotometer is not particularly limited as long as it is a known specification. However, since it can measure the difference in absorbance between the measurement sample and the control sample, the double beam type is preferable, and the spectrophotometer UV-1600PC (manufactured by Shimadzu Corporation) is preferable. ) And the like. Once installed, this spectrophotometer can be used stably for a long time. Further, the absorbance measurement temperature is not particularly limited as long as the measurement sample or the target sample is liquid, but specifically, 10 ° C. to 30 ° C. is preferable from the viewpoint of ease of handling of the measurement sample and the target sample. 15 to 30 ° C. is more preferable, and 20 to 25 ° C. is more preferable.
  本発明において、光照射の波長は、乳性食品の５０％粒子径との相関関係が回帰曲線や回帰直線などで表現できれば、特に限定されない。このとき、本発明では、光照射による吸光度と乳性食品の５０％粒子径との相関関係が明確であることから、光照射が５００ｎｍ～１１００ｎｍ（近赤外線領域）の波長であることが好ましく、光照射が８００ｎｍ～１１００ｎｍの波長であることがより好ましい。 に お い て In the present invention, the wavelength of light irradiation is not particularly limited as long as the correlation with the 50% particle size of the dairy food can be expressed by a regression curve, a regression line, or the like. At this time, in the present invention, since the correlation between the absorbance by light irradiation and the 50% particle size of the dairy food is clear, it is preferable that the light irradiation has a wavelength of 500 nm to 1100 nm (near infrared region), More preferably, the light irradiation has a wavelength of 800 nm to 1100 nm.
  本発明において、乳性食品の５０％粒子径は、光照射による吸光度の測定値と粒度分布測定装置による乳性食品の５０％粒子径の測定値との相関関係が明確であることから、０．１～２．５μｍであることが好ましく、０．２～２．０μｍであることがより好ましく、０．３～２．０μｍであることがさらに好ましく、０．４～２．０μｍであることがとくに好ましい。乳性食品の５０％粒子径が２．５μｍより大きいと、検量線の相関関係から外れやすく、乳性食品の５０％粒子径が０．１μｍより小さいと、実際の加工工程や製造工程で調製しにくい。 In the present invention, the 50% particle size of the dairy food is 0 because the correlation between the measured value of the absorbance by light irradiation and the measured value of the 50% particle size of the dairy food by the particle size distribution measuring device is clear. It is preferably 1 to 2.5 μm, more preferably 0.2 to 2.0 μm, further preferably 0.3 to 2.0 μm, and 0.4 to 2.0 μm. Is particularly preferred. If the 50% particle size of the dairy food is larger than 2.5 μm, it is easy to deviate from the correlation of the calibration curve. Hard to do.
  本発明において、粒度分布測定装置による５０％粒子径の測定値は、公知の原理を用いて測定できれば、特に限定されない。このとき、本発明では、５０％粒子径を簡便で安価に測定でき、汎用性も高いため、粒度分布測定装置を使用することが好ましく、レーザー回折式の粒度分布測定装置ＳＡＬＤ－２００１システム（島津製作所製）などを例示できる。この粒度分布測定装置は、いったん導入して設置すれば長期的に安定して使用できる。 に お い て In the present invention, the 50% particle diameter measured value by the particle size distribution measuring device is not particularly limited as long as it can be measured using a known principle. At this time, in the present invention, it is preferable to use a particle size distribution measuring device because the 50% particle size can be measured easily and inexpensively and has high versatility. A laser diffraction particle size distribution measuring device SALD-2001 system (Shimadzu) (Manufactured by Seisakusho) and the like. Once this particle size distribution measuring device is introduced and installed, it can be used stably for a long time.
  本発明において、粒度分布測定装置による５０％粒子径の測定値は、レーザー回折・散乱法により、乳性食品などの分散体の粒度分布を測定した結果に対して、その積算値で５０％の粒子径である。ここで、積算値で５０％の粒子径とは、粒子径の小さい方から粒子数を加算していき、全部の粒子数の５０％に到達したところの粒子径である。乳性食品のうち、牛乳や乳飲料などでは、５０％粒子径の測定値を平均脂肪球径と称することもあるが、本発明において、５０％粒子径は、平均脂肪球径の意味も包含される。 In the present invention, the measured value of the 50% particle size by the particle size distribution measuring device is 50% of the integrated value with respect to the result of measuring the particle size distribution of the dispersion such as dairy food by the laser diffraction / scattering method. The particle size. Here, the particle size of 50% in terms of the integrated value is the particle size when the number of particles is added from the smaller particle size and reaches 50% of the total number of particles. Among milk foods, in milk and milk drinks, the measured value of 50% particle diameter is sometimes referred to as average fat globule diameter. In the present invention, 50% particle diameter includes the meaning of average fat globule diameter. Is done.
  本発明において、乳性食品は、乳含有の（液状の）食品、乳由来の原料、それらの加工品などであり、特に狭義には限定されない。具体的には、牛、羊、山羊、水牛などに由来する獣乳、加工獣乳、獣乳飲料、獣乳入り清涼飲料であり、大豆などに由来する植物乳、加工植物乳、植物乳飲料、植物乳入り清涼飲料であることが好ましく、代表的に市場で流通していることから、獣乳が牛乳であり、植物乳が豆乳であることがより好ましい。なお、植物油脂とその他の原料を乳化させて構成された人工乳も、植物乳に包含される。 に お い て In the present invention, dairy foods are milk-containing (liquid) foods, milk-derived raw materials, processed products thereof, and the like, and are not particularly limited. Specifically, animal milk derived from cows, sheep, goats, buffalos, processed animal milk, animal milk drinks, soft drinks containing animal milk, plant milk derived from soybeans, processed vegetable milk, vegetable milk drinks Since it is preferably a soft drink containing vegetable milk and is typically distributed in the market, it is more preferable that animal milk is cow milk and plant milk is soy milk. In addition, artificial milk constituted by emulsifying vegetable oil and other raw materials is also included in the vegetable milk.
  本発明において、乳性食品は、例えば、牛乳の還元の度合いや加工の度合いには、特に限定されない。具体的には、生乳や生乳を殺菌処理した牛乳の他、全脂濃縮乳、全脂粉乳、部分脱脂乳、部分脱脂濃縮乳、部分脱脂粉乳、脱脂乳、脱脂濃縮乳、脱脂粉乳、クリーム、バターなどの還元乳製品にも、それらを液状に還元することで、本発明を適用できる。さらに、牛乳や乳製品を配合して必要な組成に調製した加工乳、牛乳を膜処理して各種の成分を濃縮や除去した加工乳、牛乳や乳製品や加工乳などを含めた乳飲料や乳入り清涼飲料にも、本発明を適用できる。そして、これらは、牛乳以外の獣乳や植物乳にも同様に、本発明を適用できる。 に お い て In the present invention, the dairy food is not particularly limited, for example, to the degree of milk reduction or processing. Specifically, in addition to raw milk and milk sterilized raw milk, concentrated whole milk, whole milk powder, partially skimmed milk, partially skimmed concentrated milk, partially skimmed milk powder, skimmed milk, skimmed concentrated milk, skimmed milk powder, cream, The present invention can also be applied to reduced dairy products such as butter by reducing them to liquid form. Furthermore, processed milk prepared by mixing milk and dairy products to the required composition, processed milk obtained by membrane treatment of milk to concentrate and remove various ingredients, milk drinks including milk, dairy products and processed milk, The present invention can also be applied to soft drinks containing milk. And these can apply this invention similarly to animal milk and vegetable milk other than milk.
  本発明において、乳性食品は、商品特性に合わせて、獣乳以外や植物乳以外の食品、各種の食品添加物などを任意に添加できる。ここで、例えば、食品には、珈琲、茶、果汁、糖類、高甘味度甘味料などを挙げられ、食品添加物には、安定剤、増粘剤、防腐剤、カルシウムなどのミネラル類、香料などを挙げられる。 に お い て In the present invention, the dairy food can be arbitrarily added with foods other than animal milk or vegetable milk, various food additives, etc., in accordance with product characteristics. Here, for example, food includes salmon, tea, fruit juice, sugar, high-intensity sweetener, and the like, and food additives include stabilizers, thickeners, preservatives, minerals such as calcium, and flavors. Etc.
　本発明は、乳性食品の５０％粒子径と、光照射による吸光度の測定値との間に相関関係が存在していることを見出した。つまり、従来の粒度分布測定装置による少なくとも２つの乳性食品の５０％粒子径を得るステップと、当該乳性食品の光照射による吸光度を得るステップと、前記５０％粒子径と前記吸光度との相関関係を割り出すステップと、当該相関関係を利用して未知の乳性食品の５０％粒子径の簡易測定方法。ここでいう「相関関係」とは、前記吸光度と５０％粒子径との間に、例えば、関数（一次、二次等）関係が成り立つことをいう。その相関関係によって、未知の５０％粒子径を吸光度で簡単に計ることができる。また割り出す方法の具体的な方法は、サンプリングとして、少なくとも２つのサンプルを選び、前記のように粒度分布測定装置を用いてその５０％粒子径を測定し、５０％粒子径が得られたサンプルに光照射をあてることで得られる吸光度値と当該５０％粒子径値とを線形最小自乗法を適用し、予め数式と換算係数を算出する方法が例としてあげられる。これによって、乳性食品の５０％粒子径と、光照射による吸光度の測定値との間に比例関係（一次関数：吸光度＝ａ×粒子径＋ｂ（後述する表２等を参照））という相関関係が成り立つ。また、同じ理屈で、他の相関関係、例えば、二次関数等を導き出すこともできる。 The present invention has found that there is a correlation between the 50% particle size of dairy foods and the absorbance measured by light irradiation. That is, obtaining a 50% particle size of at least two dairy foods using a conventional particle size distribution measuring device, obtaining an absorbance of the dairy food by light irradiation, and correlation between the 50% particle size and the absorbance. A step of determining the relationship, and a simple measurement method of 50% particle size of an unknown milk food using the correlation. “Correlation” as used herein means that, for example, a function (primary, secondary, etc.) relationship is established between the absorbance and the 50% particle size. Due to the correlation, an unknown 50% particle size can be easily measured by absorbance. In addition, a specific method of determining is to select at least two samples as sampling, measure the 50% particle diameter using the particle size distribution measuring apparatus as described above, and obtain a sample having a 50% particle diameter. An example is a method in which a linear least square method is applied to the absorbance value obtained by light irradiation and the 50% particle size value, and a mathematical formula and a conversion coefficient are calculated in advance. Accordingly, there is a proportional relationship between the 50% particle size of the dairy food and the measured absorbance value by light irradiation (linear function: absorbance = a × particle size + b (see Table 2 and the like described later)). Holds. Also, with the same reason, other correlations such as quadratic functions can be derived.
  本発明において、乳性食品の５０％粒子径は、例えば、光照射による吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値との相関関係に対して、非線形最小自乗法や線形最小自乗法などの公知の近似方法を適用する。そして、その相関関係を数式などで予め算出しておき、実際に測定試料や対照試料の吸光度を測定し、その相関関係の数式などに当てはめて算出できる。ただし、乳性食品の５０％粒子径は、光照射による吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値との相関関係を利用して算出すれば、特に限定されない。具体的には、光照射が５００ｎｍ～１１００ｎｍの波長である吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値との相関関係を検量線や関数電卓などで算出してから、線形最小自乗法を適用し、予め数式と換算係数を算出する。
そして、実際に測定試料や対照試料の吸光度を測定し、予め算出した数式と換算係数を適用して、乳性食品の５０％粒子径を算出する。なお、これら検量線などの線形最小自乗法の相関係数（Ｒ2）では、０．９０以上が好ましく、０．９３以上がより好ましく、０．９５以上がさらに好ましい。線形最小自乗法の相関係数が０．９０未満では、検量線の精度が落ち、乳性食品の５０％粒子径を精度良く算出できなくなる虞がある。 In the present invention, the 50% particle size of the dairy food is determined by, for example, nonlinear least square method or linearity with respect to the correlation between the measured value of absorbance by light irradiation and the measured value of 50% particle size by a particle size distribution measuring device. A known approximation method such as a least square method is applied. Then, the correlation can be calculated in advance using a mathematical formula or the like, and the absorbance of the measurement sample or the control sample can be actually measured and applied to the correlation mathematical formula or the like. However, the 50% particle size of the dairy food is not particularly limited as long as it is calculated using the correlation between the measured value of absorbance by light irradiation and the measured value of 50% particle size by a particle size distribution measuring device. Specifically, the correlation between the measured value of absorbance at which light irradiation is at a wavelength of 500 nm to 1100 nm and the measured value of 50% particle size by a particle size distribution measuring device is calculated using a calibration curve or a scientific calculator, and then linear The least square method is applied, and mathematical formulas and conversion coefficients are calculated in advance.
Then, the absorbance of the measurement sample and the control sample is actually measured, and the 50% particle size of the dairy food is calculated by applying the mathematical formula and the conversion factor calculated in advance. Note that the correlation coefficient (R 2 ) of the linear least square method such as a calibration curve is preferably 0.90 or more, more preferably 0.93 or more, and further preferably 0.95 or more. If the correlation coefficient of the linear least squares method is less than 0.90, the accuracy of the calibration curve is lowered, and there is a possibility that the 50% particle diameter of dairy foods cannot be accurately calculated.
  本発明において、吸光度測定装置として、分光光度計ＵＶ－１６００ＰＣ（島津製作所製）を、粒度分布測定装置として、レーザー回折式の粒度分布測定装置ＳＡＬＤ－２００１システム（島津製作所製）を例示している。ただし、本発明の実施の時点では、これらの装置のリニューアルやバージョンアップなどに伴い、これらの装置が必ずしも存在しないかも知れない。しかしながら、実際に流通や販売している同様の機能を備えた代替装置であれば、製造元、機種、型番などに関わらず、本発明を実施できることは当然である。
すなわち、光照射による吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値を、それらの代替装置で測定し、それぞれの測定値の相関関係を利用して、乳性食品の５０％粒子径を算出できることは言うまでもない。 In the present invention, the spectrophotometer UV-1600PC (manufactured by Shimadzu Corporation) is exemplified as the absorbance measuring apparatus, and the laser diffraction particle size distribution measuring apparatus SALD-2001 system (manufactured by Shimadzu Corporation) is exemplified as the particle size distribution measuring apparatus. . However, at the time of implementation of the present invention, these devices may not necessarily exist due to renewal or version upgrade of these devices. However, it is a matter of course that the present invention can be implemented regardless of the manufacturer, model, model number, etc., as long as it is an alternative device having the same function that is actually distributed or sold.
That is, the measured value of absorbance by light irradiation and the measured value of 50% particle size by the particle size distribution measuring device are measured by these alternative devices, and the correlation between the measured values is used to determine 50% of milk food. Needless to say, the particle size can be calculated.
  以下では、実施例を挙げて、本発明をさらに詳細に説明するが、本発明は、これにより限定されない。 In the following, the present invention will be described in more detail with reference to examples, but the present invention is not limited thereto.
（試験例１）
  生乳（無脂乳固形分：８．７％、乳脂肪分：４．１％）を３ｋｇで用意し、ステンレス製の小型容器内で攪拌しながら、１０℃から６０℃まで加熱した後に、卓上均質機（ＮＳ１００１、Ｎｉｒｏ  Ｓｏａｖｉ社製）を用いて、表１に示した５種類の圧力で均質化処理した。これら５種類の未加熱乳を耐熱容器内に分注してから、オートクレーブを用いて、１１０℃、１分間で加熱した後に、氷水で１０℃以下に冷却し、５種類の加熱乳（牛乳）を調製した（試料１～５）。これらの試料１～５を１００倍に希釈してから、分光光度計（ＵＶ－１６００ＰＣ、島津製作所社製）を用いて、光照射の波長が４００ｎｍ、５００ｎｍ、６００ｎｍ、７００ｎｍ、８００ｎｍ、９００ｎｍ、１０００ｎｍ、１１００ｎｍの吸光度を測定すると共に、粒度分布計（ＳＡＬＤ－２００１、島津製作所社製）を用いて、５０％粒子径を測定し、その結果を表１に示した。また、各波長における吸光度と、５０％粒子径との相関関係を、一次直線的に近似し、その相関係数などを表２に示した。 (Test Example 1)
Prepare raw milk (non-fat milk solid content: 8.7%, milk fat content: 4.1%) at 3kg, heat from 10 ° C to 60 ° C while stirring in a small stainless steel container, Using a homogenizer (NS1001, manufactured by Niro Soavi), homogenization treatment was performed at five pressures shown in Table 1. After dispensing these 5 types of unheated milk in a heat-resistant container, using an autoclave, heating at 110 ° C. for 1 minute, cooling to 10 ° C. or less with ice water, and then 5 types of heated milk (milk) Were prepared (Samples 1 to 5). After diluting these samples 1 to 5 100 times, using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation), the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm. Absorbance at 1100 nm was measured, and a 50% particle size was measured using a particle size distribution analyzer (SALD-2001, manufactured by Shimadzu Corporation). The results are shown in Table 1. Further, the correlation between the absorbance at each wavelength and the 50% particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 2.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
  表２より、波長が８００ｎｍから１１００ｎｍまで、５０％粒子径が０．４６μｍから１．９７μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が７００ｎｍで、５０％粒子径が０．４６μｍから１．３９μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が５００ｎｍから６００ｎｍまで、５０％粒子径が０．４６μｍから１．０３μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が４００ｎｍの場合、吸光度と５０％粒子径との相関関係は比例しておらず、一次直線的に近似できなかった。 From Table 2, when the wavelength is from 800 nm to 1100 nm and the 50% particle diameter is from 0.46 μm to 1.97 μm, the correlation between the absorbance and the 50% particle diameter is proportional. I was able to approximate. When the wavelength was 700 nm and the 50% particle diameter was 0.46 μm to 1.39 μm, the correlation between the absorbance and the 50% particle diameter was proportional, and it could be approximated linearly by the method of least squares. When the wavelength is from 500 nm to 600 nm and the 50% particle size is from 0.46 μm to 1.03 μm, the correlation between the absorbance and the 50% particle size is proportional, and can be approximated linearly by the least square method. It was. When the wavelength was 400 nm, the correlation between the absorbance and the 50% particle size was not proportional and could not be approximated linearly.
（試験例２）
  試験例１で調製した加熱乳（試料１）を４０ｇ、市販の無糖タイプの珈琲飲料（「セブンプレミアム  無糖コーヒー」）を１６ｇ、砂糖を５．６ｇ、及び原料水を１８．４ｇで用意し、それぞれを混合した。この混合物を耐熱容器内に分注してから、オートクレーブを用いて、１１０℃、１分間で加熱した後に、氷水で１０℃以下に冷却し、珈琲乳飲料を調製した（試料６）。実施例１で調製した加熱乳（試料２～５）でも、前記と同様にして、珈琲乳飲料を調製した（試料７～１０）。これらの試料６～１０を１００倍に希釈してから、分光光度計（ＵＶ－１６００ＰＣ、島津製作所社製）を用いて、光照射の波長が４００ｎｍ、５００ｎｍ、６００ｎｍ、７００ｎｍ、８００ｎｍ、９００ｎｍ、１０００ｎｍ、１１００ｎｍの吸光度を測定すると共に、粒度分布計（ＳＡＬＤ－２００１、島津製作所社製）を用いて、５０％粒子径を測定し、その結果を表３に示した。また、各波長における吸光度と、５０％粒子径との相関関係を、一次直線的に近似し、その相関係数などを表４に示した。 (Test Example 2)
40 g of heated milk prepared in Test Example 1 (Sample 1), 16 g of a commercially available sugar-free koji beverage (“Seven Premium Unsweetened Coffee”), 5.6 g of sugar, and 18.4 g of raw water are prepared. And mixed each. This mixture was dispensed into a heat-resistant container and then heated at 110 ° C. for 1 minute using an autoclave, and then cooled to 10 ° C. or lower with ice water to prepare a milk drink (Sample 6). In the same manner as described above, milk drinks were also prepared for the heated milk prepared in Example 1 (Samples 2 to 5) (Samples 7 to 10). After these samples 6 to 10 were diluted 100 times, the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation). Absorbance at 1100 nm was measured, and a 50% particle size was measured using a particle size distribution meter (SALD-2001, manufactured by Shimadzu Corporation). The results are shown in Table 3. Further, the correlation between the absorbance at each wavelength and the 50% particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 4.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
  表４より、波長が８００ｎｍから１１００ｎｍまで、５０％粒子径が０．４６μｍから１．９７μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が５００ｎｍから７００ｎｍまで、５０％粒子径が０．４６μｍから１．３９μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が４００ｎｍの場合、吸光度と５０％粒子径との相関関係は比例しておらず、一次直線的に近似できなかった。すなわち、吸光度と５０％粒子径との相関関係について、加熱乳（牛乳）で確認された傾向が、珈琲成分などを添加した珈琲乳飲料でも確認されることが分かった。 From Table 4, when the wavelength is from 800 nm to 1100 nm and the 50% particle diameter is from 0.46 μm to 1.97 μm, the correlation between the absorbance and the 50% particle diameter is proportional. I was able to approximate. When the wavelength is from 500 nm to 700 nm and the 50% particle diameter is from 0.46 μm to 1.39 μm, the correlation between the absorbance and the 50% particle diameter is proportional, and can be approximated linearly by the least square method. It was. When the wavelength was 400 nm, the correlation between the absorbance and the 50% particle size was not proportional and could not be approximated linearly. That is, it was found that the correlation between the absorbance and the 50% particle diameter was confirmed in heated milk (milk) even in a milk drink to which a strawberry component or the like was added.
（試験例３）
  脱脂粉乳を２７１．８ｇ、無塩バターを１２７．５ｇ、原料水を２６００．７ｇで用意し、それぞれを混合した。この調合乳（無脂乳固形分：８．７％、乳脂肪分：３．６％）をステンレス製の大型容器内で攪拌しながら、１０℃から６０℃まで加熱した後に、卓上均質機（ＮＳ１００１、Ｎｉｒｏ  Ｓｏａｖｉ社製）を用いて、表５に示した５種類の圧力で均質化処理した。これら５種類の未加熱加工乳を耐熱容器内に分注してから、オートクレーブを用いて、１１０℃、１分間で加熱した後に、氷水で１０℃以下に冷却し、５種類の加熱加工乳（加工乳）を調製した（試料１１～１５）。これらの試料１１～１５を１００倍に希釈してから、分光光度計（ＵＶ－１６００ＰＣ、島津製作所社製）を用いて、光照射の波長が４００ｎｍ、５００ｎｍ、６００ｎｍ、７００ｎｍ、８００ｎｍ、９００ｎｍ、１０００ｎｍ、１１００ｎｍの吸光度を測定すると共に、粒度分布計（ＳＡＬＤ－２００１、島津製作所社製）を用いて、５０％粒子径を測定し、その結果を表５に示した。また、各波長における吸光度と、５０％粒子径との相関関係を、一次直線的に近似し、その相関係数などを表６に示した。 (Test Example 3)
271.8 g of skim milk powder, 127.5 g of unsalted butter, and 2600.7 g of raw water were prepared and mixed. This mixed milk (non-fat milk solid content: 8.7%, milk fat content: 3.6%) was heated from 10 ° C to 60 ° C while stirring in a large stainless steel container, NS1001 (manufactured by Niro Soavi) was used for homogenization at five pressures shown in Table 5. After dispensing these 5 types of unheated processed milk into a heat-resistant container, using an autoclave, heating at 110 ° C. for 1 minute, cooling to 10 ° C. or less with ice water, Processed milk) (samples 11 to 15). After diluting these samples 11 to 15 100 times, the wavelength of light irradiation was 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation). The absorbance at 1100 nm was measured, and a 50% particle size was measured using a particle size distribution meter (SALD-2001, manufactured by Shimadzu Corporation). The results are shown in Table 5. Further, the correlation between the absorbance at each wavelength and the 50% particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 6.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000006
Figure JPOXMLDOC01-appb-T000006
  表６より、波長が６００ｎｍから１１００ｎｍまで、５０％粒子径が０．５４μｍから１．７４μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が５００ｎｍで、５０％粒子径が０．５４μｍから１．４２μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。波長が５００ｎｍから１１００ｎｍまで、５０％粒子径が２．５９μｍの場合、吸光度と５０％粒子径との相関関係は比例しておらず、一次直線的に近似できなかった。波長が４００ｎｍの場合、吸光度と５０％粒子径との相関関係は比例しておらず、一次直線的に近似できなかった。すなわち、吸光度と５０％粒子径との相関関係について、加熱乳（牛乳）で確認された傾向が、還元乳原料で調製した加工乳でも確認されることが分かった。 From Table 6, when the wavelength is from 600 nm to 1100 nm and the 50% particle diameter is from 0.54 μm to 1.74 μm, the correlation between the absorbance and the 50% particle diameter is proportional. I was able to approximate. When the wavelength was 500 nm and the 50% particle size was from 0.54 μm to 1.42 μm, the correlation between the absorbance and the 50% particle size was proportional, and could be approximated linearly by the least square method. When the wavelength was 500 nm to 1100 nm and the 50% particle size was 2.59 μm, the correlation between the absorbance and the 50% particle size was not proportional and could not be approximated linearly. When the wavelength was 400 nm, the correlation between the absorbance and the 50% particle size was not proportional and could not be approximated linearly. That is, it was found that the correlation between absorbance and 50% particle diameter was confirmed in heated milk (milk) and also in processed milk prepared from reduced milk raw materials.
（試験例４）
  生乳を５２６８０ｇ、脱脂濃縮乳を２０７０ｇ、原料水を５２５０ｇで用意し、それぞれを混合した。この調合乳（無脂乳固形分：８．８％、乳脂肪分：３．６％）をタンク内で攪拌しながら、１０℃から６０℃まで加熱した後に、均質機（ホモゲナイザー）を用いて、表７に示した３種類の圧力で均質化処理した。これら３種類の未加熱加工乳について、プレート式熱交換機を用いて、８５℃で予熱してから、１３０℃、２秒間で加熱した後に、１０℃以下に冷却し、３種類の加熱加工乳（加工乳）を調製した（試料１６～１８）。これらの試料１６～１８を１００倍に希釈してから、分光光度計（ＵＶ－１６００ＰＣ、島津製作所社製）を用いて、光照射の波長が８００ｎｍ、８５０ｎｍ、９００ｎｍ、１０００ｎｍ、１１００ｎｍの吸光度を測定すると共に、粒度分布計（ＳＡＬＤ－２００１、島津製作所社製）を用いて、５０％粒子径を測定し、その結果を表７に示した。また、各波長における吸光度と、５０％平均粒子径との相関関係を、一次直線的に近似し、その相関係数などを表８に示した。 (Test Example 4)
52680 g of raw milk, 2070 g of nonfat concentrated milk, and 5250 g of raw water were prepared and mixed. This mixed milk (non-fat milk solid content: 8.8%, milk fat content: 3.6%) was heated from 10 ° C. to 60 ° C. with stirring in a tank, and then used with a homogenizer (homogenizer). Homogenization was performed at three types of pressure shown in Table 7. These three types of unheated processed milk are preheated at 85 ° C. using a plate heat exchanger, heated at 130 ° C. for 2 seconds, cooled to 10 ° C. or lower, and then heated to three types of heated processed milk ( Processed milk) (samples 16-18). After diluting these samples 16 to 18 100 times, using a spectrophotometer (UV-1600PC, manufactured by Shimadzu Corporation), the absorbance at light irradiation wavelengths of 800 nm, 850 nm, 900 nm, 1000 nm, and 1100 nm was measured. At the same time, a particle size distribution meter (SALD-2001, manufactured by Shimadzu Corporation) was used to measure the 50% particle size. The results are shown in Table 7. Further, the correlation between the absorbance at each wavelength and the 50% average particle diameter was approximated linearly, and the correlation coefficient and the like are shown in Table 8.
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000008
Figure JPOXMLDOC01-appb-T000008
  表８より、波長が８００ｎｍから１１００ｎｍまで、５０％粒子径が０．６８μｍから１．２９μｍまでの場合、吸光度と５０％粒子径との相関関係が比例しており、最小自乗法により、一次直線的に近似できた。 From Table 8, when the wavelength is from 800 nm to 1100 nm and the 50% particle diameter is from 0.68 μm to 1.29 μm, the correlation between the absorbance and the 50% particle diameter is proportional. I was able to approximate.
  本発明では、乳性食品の５０％粒子径と、光照射による吸光度の測定値との間に相関関係が存在していることを見出し、ロケーションや装置の制限が少なく、安定した吸光度が得られることから、粒度分布測定装置のような大掛かりで特殊な設備を使用せずに、乳性食品の５０％粒子径を簡便で安価に測定する方法を提供できる。そして、本発明では、汎用性の高い分光光度計を使用して、乳性食品の５０％粒子径を簡易的に測定できるため、乳性食品の品質（風味、食感、物性など）を容易に管理・制御・設計などする方法を提供できる。 In the present invention, it is found that there is a correlation between the 50% particle size of dairy foods and the measurement value of absorbance by light irradiation, and there are few restrictions on locations and devices, and stable absorbance can be obtained. Therefore, it is possible to provide a simple and inexpensive method for measuring the 50% particle size of dairy foods without using a large and special equipment such as a particle size distribution measuring apparatus. And in this invention, since the 50% particle diameter of dairy foods can be simply measured using a highly versatile spectrophotometer, the quality (flavor, texture, physical properties, etc.) of dairy foods is easy. Can provide management, control and design methods.

Claims (8)

  1. 光照射による吸光度の測定値と粒度分布測定装置による５０％粒子径の測定値との相関関係を利用することを特徴とする乳性食品の５０％粒子径の簡易測定方法。 A simple method for measuring the 50% particle size of a dairy food, which uses a correlation between a measured value of absorbance by light irradiation and a measured value of 50% particle size by a particle size distribution measuring device.
  2. 相関関係が比例関係であることを特徴とする請求項１記載の乳性食品の５０％粒子径の簡易測定方法。 2. The method for easily measuring 50% particle size of dairy foods according to claim 1, wherein the correlation is a proportional relationship.
  3. 光照射が５００ｎｍ～１１００ｎｍの波長であることを特徴とする請求項１又は２記載の乳性食品の５０％粒子径の簡易測定方法。 3. The method for easily measuring a 50% particle diameter of a dairy food according to claim 1, wherein the light irradiation has a wavelength of 500 nm to 1100 nm.
  4. 光照射が８００ｎｍ～１１００ｎｍの波長であることを特徴とする請求項１～３の何れか１項記載の乳性食品の５０％粒子径の簡易測定方法。 The simple method for measuring the 50% particle size of a dairy food according to any one of claims 1 to 3, wherein the light irradiation has a wavelength of 800 nm to 1100 nm.
  5. 乳性食品の５０％粒子径が０．１～２．０μｍであることを特徴とする請求項１～４の何れか１項記載の乳性食品の５０％粒子径の簡易測定方法。 The simple method for measuring the 50% particle diameter of a dairy food according to any one of claims 1 to 4, wherein the 50% particle diameter of the dairy food is 0.1 to 2.0 µm.
  6. 乳性食品が獣乳、加工獣乳、獣乳飲料、獣乳入り清涼飲料、植物乳、加工植物乳、植物乳飲料、植物乳入り清涼飲料であることを特徴とする請求項１～５の何れか１項記載の乳性食品の５０％粒子径の簡易測定方法。 The dairy food is animal milk, processed animal milk, animal milk drink, soft drink with animal milk, vegetable milk, processed vegetable milk, vegetable milk drink, or soft drink with vegetable milk. The simple measuring method of the 50% particle diameter of the dairy food of any one of Claims 1.
  7. 獣乳が牛乳であり、植物乳が豆乳であることを特徴とする請求項６記載の乳性食品の５０％粒子径の簡易測定方法。 The simple method for measuring a 50% particle size of a dairy food according to claim 6, wherein the animal milk is cow milk and the plant milk is soy milk.
  8. 吸光度を分光光度計で測定することを特徴とする請求項１～７の何れか１項記載の乳性食品の５０％粒子径の簡易測定方法。 The simple method for measuring the 50% particle size of a dairy food according to any one of claims 1 to 7, wherein the absorbance is measured with a spectrophotometer.
PCT/JP2013/054260 2012-02-21 2013-02-21 Simple method for measuring median particle size of lactic food WO2013125612A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2014500750A JP6196610B2 (en) 2012-02-21 2013-02-21 Simple measurement method for 50% particle size of dairy foods
CN201380010383.4A CN104136906A (en) 2012-02-21 2013-02-21 Simple method for measuring median particle size of lactic food

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2012-035375 2012-02-21
JP2012035375 2012-02-21

Publications (1)

Publication Number Publication Date
WO2013125612A1 true WO2013125612A1 (en) 2013-08-29

Family

ID=49005792

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2013/054260 WO2013125612A1 (en) 2012-02-21 2013-02-21 Simple method for measuring median particle size of lactic food

Country Status (3)

Country Link
JP (1) JP6196610B2 (en)
CN (1) CN104136906A (en)
WO (1) WO2013125612A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015059775A (en) * 2013-09-17 2015-03-30 ポーラ化成工業株式会社 Evaluation method and production method of emulsion cosmetics

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0231133A (en) * 1988-07-20 1990-02-01 Shimadzu Corp Apparatus for measuring refractive index of particle
JPH0315741A (en) * 1989-06-13 1991-01-24 Satake Eng Co Ltd Near infrared spectrochemical analysis
JP2004217761A (en) * 2003-01-14 2004-08-05 Asahi Kasei Chemicals Corp Core/shell type acrylic polymer particles
JP2007023384A (en) * 2005-07-08 2007-02-01 Dai Ichi Pure Chem Co Ltd Method for adjusting diameter of colloidal gold particle and colloidal gold solution
JP2007077000A (en) * 2005-08-17 2007-03-29 Takeda Chem Ind Ltd Method for monitoring crystallization process of compound and method for producing crystal
JP2011179074A (en) * 2010-03-01 2011-09-15 Utsunomiya Univ Gold nanoparticle, and method for producing the same
JP2012177679A (en) * 2011-01-31 2012-09-13 Institute Of National Colleges Of Technology Japan Granularity representative value estimation device and granularity representative value estimation method

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1438631A (en) * 1972-08-04 1976-06-09 Parsons & Co Sir Howard G Analysis of emulsions and suspensions
IN152513B (en) * 1978-12-06 1984-02-04 Foss Electric As N
JPH0820355B2 (en) * 1988-11-24 1996-03-04 元二 神保 Particle size measurement method
SE507486C3 (en) * 1991-09-12 1998-07-13 Valmet Automation Kajaani Ltd Method and apparatus for saturating fiber properties with near-infrared spectroscopy
DK171927B1 (en) * 1995-02-10 1997-08-11 Slagteriernes Forskningsinst Method and apparatus for determining the particle size of a food or feed material
EP1935983B1 (en) * 1997-05-05 2011-06-22 ChemoMetec A/S Method for determination of biological particles in blood
JP3741396B2 (en) * 1997-06-26 2006-02-01 雪印乳業株式会社 Nutrition drink and its production method
JP4263304B2 (en) * 1999-04-12 2009-05-13 雪印乳業株式会社 Apparatus and method for measuring fat concentration in cream
JP2001075420A (en) * 1999-09-08 2001-03-23 Ricoh Co Ltd Image forming device
JP4143349B2 (en) * 2002-07-22 2008-09-03 株式会社堀場製作所 Particle size distribution measuring method, particle size distribution measuring device, and particle size distribution measuring device measurement program
JP2005291704A (en) * 2003-11-10 2005-10-20 New Industry Research Organization Visible light/near infrared spectral analysis method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0231133A (en) * 1988-07-20 1990-02-01 Shimadzu Corp Apparatus for measuring refractive index of particle
JPH0315741A (en) * 1989-06-13 1991-01-24 Satake Eng Co Ltd Near infrared spectrochemical analysis
JP2004217761A (en) * 2003-01-14 2004-08-05 Asahi Kasei Chemicals Corp Core/shell type acrylic polymer particles
JP2007023384A (en) * 2005-07-08 2007-02-01 Dai Ichi Pure Chem Co Ltd Method for adjusting diameter of colloidal gold particle and colloidal gold solution
JP2007077000A (en) * 2005-08-17 2007-03-29 Takeda Chem Ind Ltd Method for monitoring crystallization process of compound and method for producing crystal
JP2011179074A (en) * 2010-03-01 2011-09-15 Utsunomiya Univ Gold nanoparticle, and method for producing the same
JP2012177679A (en) * 2011-01-31 2012-09-13 Institute Of National Colleges Of Technology Japan Granularity representative value estimation device and granularity representative value estimation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015059775A (en) * 2013-09-17 2015-03-30 ポーラ化成工業株式会社 Evaluation method and production method of emulsion cosmetics

Also Published As

Publication number Publication date
CN104136906A (en) 2014-11-05
JPWO2013125612A1 (en) 2015-07-30
JP6196610B2 (en) 2017-09-13

Similar Documents

Publication Publication Date Title
Wherry et al. Use of acid whey protein concentrate as an ingredient in nonfat cup set-style yogurt
RU2453128C2 (en) Whey protein denaturation method
Beliciu et al. The effect of commercial sterilization regimens on micellar casein concentrates
JP5421123B2 (en) Novel drink yogurt and method for producing the same
Fiol et al. Introduction of a new family of ice creams
JP6600622B2 (en) Method for producing weakly acidic milk beverage
CA2606555C (en) Method for the manufacturing of soy and milk protein-based preparations having a high total protein content
WO2015111357A1 (en) Acidic lactic beverage and method for producing same
Kumbár et al. Viscosity and analytical differences between raw milk and UHT milk of Czech cows
Singh et al. Comparison of ultra high temperature (UHT) stability of high protein milk dispersions prepared from milk protein concentrate (MPC) and conventional low heat skimmed milk powder (SMP)
Caro et al. Compositional, functional and sensory characteristics of selected Mexican cheeses
Cheng et al. Effects of milk fat, casein, and serum protein concentrations on sensory properties of milk-based beverages
Szkolnicka et al. Buttermilk ice cream—New method for buttermilk utilization
WO2011099876A1 (en) Dairy product and process
Patel et al. Milk protein concentrates: Manufacturing and applications
CN103828931B (en) Fruit-vegetable processed cheese spread and preparation method thereof
De Bassi et al. Evaluation of physicochemical, microbiological and sensorial characteristics of fermented milk beverages with buttermilk addition
CN114173568A (en) Dairy product and process
JP6196610B2 (en) Simple measurement method for 50% particle size of dairy foods
Baldwin et al. Milk powder
JP7128912B2 (en) Lactose-free dairy
RU2458515C1 (en) Buttermilk beverage production method
Pascual Effects of different types of milk fat globule membrane materials on the physical and rheological characteristics of set yoghurts
Sohany et al. Effect of garlic paste on the physicochemical attributes of cheese
WO2016076326A1 (en) Method for manufacturing weakly acidic milk drink

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 13752052

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2014500750

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 13752052

Country of ref document: EP

Kind code of ref document: A1