JP2018136151A - Determination method and production method for oil and fat composition - Google Patents
Determination method and production method for oil and fat composition Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 173
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 239000003925 fat Substances 0.000 claims abstract description 365
- 239000003921 oil Substances 0.000 claims abstract description 349
- 230000005284 excitation Effects 0.000 claims abstract description 50
- 235000019198 oils Nutrition 0.000 claims description 328
- 238000011088 calibration curve Methods 0.000 claims description 49
- 238000002156 mixing Methods 0.000 claims description 40
- 238000005259 measurement Methods 0.000 claims description 20
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 20
- 239000008158 vegetable oil Substances 0.000 claims description 16
- 235000019197 fats Nutrition 0.000 description 241
- 239000010462 extra virgin olive oil Substances 0.000 description 42
- 235000021010 extra-virgin olive oil Nutrition 0.000 description 42
- 239000010464 refined olive oil Substances 0.000 description 20
- 235000012424 soybean oil Nutrition 0.000 description 17
- 239000003549 soybean oil Substances 0.000 description 17
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- 235000014113 dietary fatty acids Nutrition 0.000 description 6
- 229930195729 fatty acid Natural products 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 150000004665 fatty acids Chemical class 0.000 description 6
- 238000004817 gas chromatography Methods 0.000 description 5
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- 239000002600 sunflower oil Substances 0.000 description 4
- AKYHKWQPZHDOBW-UHFFFAOYSA-N (5-ethenyl-1-azabicyclo[2.2.2]octan-7-yl)-(6-methoxyquinolin-4-yl)methanol Chemical compound OS(O)(=O)=O.C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 AKYHKWQPZHDOBW-UHFFFAOYSA-N 0.000 description 3
- 239000001576 FEMA 2977 Substances 0.000 description 3
- 235000019487 Hazelnut oil Nutrition 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- LOUPRKONTZGTKE-UHFFFAOYSA-N cinchonine Natural products C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-UHFFFAOYSA-N 0.000 description 3
- 235000012343 cottonseed oil Nutrition 0.000 description 3
- 239000002385 cottonseed oil Substances 0.000 description 3
- 239000010468 hazelnut oil Substances 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 229960003110 quinine sulfate Drugs 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 235000018330 Macadamia integrifolia Nutrition 0.000 description 2
- 240000000912 Macadamia tetraphylla Species 0.000 description 2
- 235000003800 Macadamia tetraphylla Nutrition 0.000 description 2
- 235000019485 Safflower oil Nutrition 0.000 description 2
- 235000019864 coconut oil Nutrition 0.000 description 2
- 239000003240 coconut oil Substances 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 239000010466 nut oil Substances 0.000 description 2
- 235000008390 olive oil Nutrition 0.000 description 2
- 239000004006 olive oil Substances 0.000 description 2
- 239000010461 other edible oil Substances 0.000 description 2
- 235000005713 safflower oil Nutrition 0.000 description 2
- 239000003813 safflower oil Substances 0.000 description 2
- 235000011803 sesame oil Nutrition 0.000 description 2
- 239000008159 sesame oil Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 240000002791 Brassica napus Species 0.000 description 1
- 235000004977 Brassica sinapistrum Nutrition 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 244000299461 Theobroma cacao Species 0.000 description 1
- 235000005764 Theobroma cacao ssp. cacao Nutrition 0.000 description 1
- 235000005767 Theobroma cacao ssp. sphaerocarpum Nutrition 0.000 description 1
- 235000019498 Walnut oil Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 235000021324 borage oil Nutrition 0.000 description 1
- 235000014121 butter Nutrition 0.000 description 1
- 235000001046 cacaotero Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000010495 camellia oil Substances 0.000 description 1
- 235000019519 canola oil Nutrition 0.000 description 1
- 239000000828 canola oil Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000008162 cooking oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 239000008169 grapeseed oil Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 235000021388 linseed oil Nutrition 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 235000021243 milk fat Nutrition 0.000 description 1
- 239000003346 palm kernel oil Substances 0.000 description 1
- 235000019865 palm kernel oil Nutrition 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 239000008171 pumpkin seed oil Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- 239000003760 tallow Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
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Landscapes
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
本発明は、油脂組成物の判定方法及び油脂組成物の製造方法に関するものである。 The present invention relates to a method for judging an oil and fat composition and a method for producing an oil and fat composition.
２種の植物油脂を所望の含量比となるように添加混合して油脂組成物を大量生産する場合、各植物油脂を添加する速度（流速）を管理して所望の含量比の油脂組成物を製造することが一般的である。 When adding and mixing two kinds of vegetable fats and oils so as to obtain a desired content ratio and mass-producing the oil and fat composition, the rate (flow rate) at which each vegetable fat and oil is added is controlled to obtain the fat and oil composition having the desired content ratio. It is common to manufacture.
しかし、流速を管理して植物油脂を添加しているため誤差が生じやすく、製造された油脂組成物中の各植物油脂の含量比が所望の含量比から外れてしまうことがある。 However, since the vegetable oil is added by controlling the flow rate, an error is likely to occur, and the content ratio of each vegetable oil in the produced oil composition may deviate from the desired content ratio.
そこで、製造された油脂組成物中の各植物油脂の含量比を算出して、算出された含量比が所望の含量比を外れている場合には、所望の含量比を下回っている方の油脂の添加量を増やす（流速をアップする）、及び／又は所望の含量比を超えている方の油脂の添加量を減らす（流速をダウンする）ことにより調整を行なっている。油脂組成物中の各植物油脂の含量比は、油脂組成物の脂肪酸組成をガスクロマトグラフィーを使用して分析すること等により算出できる（例えば、特許文献１参照）。 Therefore, the content ratio of each vegetable fat / oil in the produced fat / oil composition is calculated, and when the calculated content ratio is out of the desired content ratio, the fat / oil that is lower than the desired content ratio is calculated. Adjustment is performed by increasing the amount of oil added (increasing the flow rate) and / or decreasing the amount of oil or fat that exceeds the desired content ratio (decreasing the flow rate). The content ratio of each vegetable fat / oil in the fat / oil composition can be calculated by analyzing the fatty acid composition of the fat / oil composition using gas chromatography (see, for example, Patent Document 1).
しかし、ガスクロマトグラフィー等を使用した従来の算出方法では、脂肪酸組成が類似の油脂の場合、精度が十分でなく、所望の含量比から外れた油脂組成物が製造されてしまうことがある。また、測定に時間がかかるため、製造効率も悪くなる。 However, in the conventional calculation method using gas chromatography or the like, in the case of fats and oils having a similar fatty acid composition, the accuracy is not sufficient, and an oil and fat composition deviating from a desired content ratio may be produced. Moreover, since measurement takes time, manufacturing efficiency also deteriorates.
また、１００％純正の油脂であるか（他の油脂が混ざっていないか）否か、あるいは産地偽装等の偽造品であるか否かの検査においてもガスクロマトグラフィー等が使用されていたが、他の油脂の混入率が低い場合（例えば、混入率が５質量％以下）や双方の油脂の脂肪酸組成が類似している場合には正確な判定が困難であった。 In addition, gas chromatography etc. was used in the inspection of whether it is 100% pure oil (other oils are not mixed) or whether it is a counterfeit product such as counterfeit production area, When the mixing rate of other fats and oils is low (for example, the mixing rate is 5% by mass or less) or when the fatty acid compositions of both fats and oils are similar, accurate determination is difficult.
従って、本発明の目的は、油脂組成物中の油脂の含量比を精度良く判定できる油脂組成物の判定方法及び所望の含量比の油脂組成物を製造できる油脂組成物の製造方法を提供することである。また、本発明の目的は、ガスクロマトグラフィーを使用する場合に比べて油脂組成物中の油脂の含量比を短時間で判定できる油脂組成物の判定方法及び所望の含量比の油脂組成物を効率よく製造できる油脂組成物の製造方法を提供することである。 Accordingly, an object of the present invention is to provide a method for determining an oil composition capable of accurately determining the content ratio of the oil in the oil composition, and a method for producing the oil composition capable of producing the oil composition having a desired content ratio. It is. In addition, the object of the present invention is to provide an oil composition determination method capable of determining the content ratio of fats and oils in the oil composition in a short time compared with the case of using gas chromatography, and an oil composition having a desired content ratio. It is providing the manufacturing method of the oil-fat composition which can be manufactured well.
また、本発明の目的は、他の油脂の混入率が低い場合や双方の油脂の脂肪酸組成が類似している場合であっても１００％純正の油脂であるか否かや偽造品であるか否かの正確な判定ができる油脂組成物の判定方法を提供することである。 In addition, the object of the present invention is whether or not it is 100% pure oil or a counterfeit product even when the mixing ratio of other oils and fats is low or the fatty acid composition of both oils and fats is similar. It is providing the determination method of the fats and oils composition which can perform accurate determination of whether or not.
本発明は、上記目的を達成するために、下記の［１］〜［７］の油脂組成物の判定方法及び下記の［８］〜［１１］の油脂組成物の製造方法を提供する。
［１］油脂Ａ、油脂Ｂ、及び前記油脂Ａと前記油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた各蛍光指紋を比較して前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で判定対象の油脂組成物の蛍光強度を測定することにより、前記判定対象の油脂組成物中の前記油脂Ａ及び／又は前記油脂Ｂの含量割合を判定する油脂組成物の判定方法。
［２］分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で前記油脂Ａと前記油脂Ｂの含量割合が既知の油脂組成物の蛍光強度を測定し、当該蛍光強度を横軸又は縦軸とし、前記油脂Ａの濃度を縦軸又は横軸として検量線を作成し、前記判定対象の油脂組成物の前記蛍光強度を前記検量線と比較することにより、前記判定対象の油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定することを特徴とする前記［１］に記載の油脂組成物の判定方法。
［３］前記油脂Ａが未精製植物油であり、前記油脂Ｂが精製植物油であることを特徴とする前記［１］又は［２］に記載の油脂組成物の判定方法。
［４］前記油脂Ａ及び前記油脂Ｂが、精製植物油であることを特徴とする前記［１］又は［２］に記載の油脂組成物の判定方法。
［５］前記各蛍光指紋を比較して前記油脂Ａに特徴的な１個以上のピーク及び前記油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて前記油脂Ａに特徴的な１個以上の前記ピークの波長（励起波長、蛍光波長）のうちの１以上で前記油脂Ａと前記油脂Ｂの含量割合が既知の油脂組成物の蛍光強度Ａを測定し、かつ前記油脂Ｂに特徴的な１個以上の前記ピークの波長（励起波長、蛍光波長）のうちの１以上で前記油脂Ａと前記油脂Ｂの含量割合が既知の油脂組成物の蛍光強度Ｂを測定し、「蛍光強度Ａの合計値／蛍光強度Ｂの合計値」の比率又は「蛍光強度Ｂの合計値／蛍光強度Ａの合計値」の比率を判定値として算出して検量線を作成し、前記油脂Ａの含量比が１００質量％であると判定できる１００質量％判定値を求め、前記判定対象の油脂組成物の前記判定値を算出して前記１００質量％判定値と比較することにより、前記判定対象の油脂組成物中の前記油脂Ａの含量が１００質量％であるか否かを判定することを特徴とする前記［１］に記載の油脂組成物の判定方法。
［６］油脂Ａを、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍ全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた第１の蛍光指紋と、前記第１の蛍光指紋の測定条件と同条件で測定して得られる判定対象の油脂組成物の第２の蛍光指紋とを比較することにより、前記油脂組成物が前記油脂Ａのみからなるか否かを判定する油脂組成物の判定方法。
［７］前記油脂Ａが精製植物油であることを特徴とする前記［６］に記載の油脂組成物の判定方法。
［８］油脂Ａと油脂Ｂとを所望の含量割合となるように添加し、混合装置により混合して油脂組成物を得る混合工程と、前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークの蛍光強度を測定することにより、前記油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定する判定工程と、前記判定された含量割合が前記所望の含量割合を外れている場合に、前記混合工程において、前記所望の含量割合を下回っている方の油脂の添加量を増やす、及び／又は前記所望の含量割合を超えている方の油脂の添加量を減らす調整工程を有することを特徴とする油脂組成物の製造方法。
［９］油脂Ａと油脂Ｂとを所望の含量割合となるように添加し、混合装置により混合して油脂組成物を得る混合工程と、下記判定方法を用いて前記油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定する判定工程と、前記判定された含量割合が前記所望の含量割合を外れている場合に、前記混合工程において、前記所望の含量割合を下回っている方の油脂の添加量を増やす、及び／又は前記所望の含量割合を超えている方の油脂の添加量を減らす調整工程を有することを特徴とする油脂組成物の製造方法。判定方法：油脂Ａ、油脂Ｂ、及び前記油脂Ａと前記油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた各蛍光指紋を比較して前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で判定対象の油脂組成物の蛍光強度を測定することにより、前記判定対象の油脂組成物中の前記油脂Ａ及び／又は前記油脂Ｂの含量割合を判定する。
［１０］前記判定方法が、分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で前記油脂Ａと前記油脂Ｂの含量割合が既知の油脂組成物の蛍光強度を測定し、当該蛍光強度を横軸又は縦軸とし、前記油脂Ａの濃度を縦軸又は横軸として検量線を作成し、前記判定対象の油脂組成物の前記蛍光強度を前記検量線と比較することにより、前記判定対象の油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定することを特徴とする前記[９]に記載の油脂組成物の製造方法。
［１１］前記混合装置が、インライン式混合装置又はバッチ式混合装置であることを特徴とする前記[８]〜[１０]のいずれか１つに記載の油脂組成物の製造方法。
In order to achieve the above object, the present invention provides a method for judging an oil composition according to the following [1] to [7] and a method for producing an oil composition according to the following [8] to [11].
[1] Two or more selected from fat and oil composition including fat and oil A, fat and oil B, and the fat and oil A and the fat and oil B, using a spectrofluorimeter, all or part of an excitation wavelength of 250 to 700 nm. One or more peaks characteristic of the fats and oils A and / or the fats and oils B are selected by comparing each fluorescent fingerprint obtained by exciting and measuring all or part of the fluorescence wavelength of 250 to 800 nm, By measuring the fluorescence intensity of the oil composition to be determined at one or more wavelengths of the peak (excitation wavelength, fluorescence wavelength) using a fluorometer, the fat A and oil A in the oil composition to be determined and // The determination method of the oil-fat composition which determines the content rate of the said oil-fat B.
[2] Using a spectrofluorometer, measure the fluorescence intensity of the fat composition having a known content ratio of the fat A and the fat B at one or more wavelengths of the peak (excitation wavelength, fluorescence wavelength), By creating a calibration curve with the fluorescence intensity as the horizontal axis or the vertical axis, the concentration of the fat A as the vertical axis or the horizontal axis, and comparing the fluorescence intensity of the determination target oil composition with the calibration curve, The determination method of the oil / fat composition according to [1], wherein the content ratio of the oil / fat A and the oil / fat B in the oil / fat composition to be determined is determined.
[3] The method for determining an oil / fat composition according to [1] or [2], wherein the oil / fat A is an unrefined vegetable oil and the oil / fat B is a refined vegetable oil.
[4] The method for judging an oil / fat composition according to [1] or [2], wherein the oil / fat A and the oil / fat B are refined vegetable oils.
[5] One or more peaks characteristic of the fat and oil A and one or more peaks characteristic of the fat and oil B are selected by comparing the fluorescent fingerprints, and the fat and oil A is selected using a spectrofluorimeter. And measuring the fluorescence intensity A of the oil / fat composition having a known content ratio of the oil / fat A and the oil / fat B at one or more of the one or more wavelengths (excitation wavelength, fluorescence wavelength) characteristic of Measure the fluorescence intensity B of an oil / fat composition having a known content ratio of the oil / fat A and the oil / fat B at one or more of the one or more wavelengths (excitation wavelength, fluorescence wavelength) characteristic of the oil / fat B Then, a calibration curve is created by calculating a ratio of “total value of fluorescence intensity A / total value of fluorescence intensity B” or ratio of “total value of fluorescence intensity B / total value of fluorescence intensity A” as a determination value, Obtain a 100% by mass judgment value that can be judged that the content ratio of the fat A is 100% by mass. Whether the content of the fat / oil A in the determination target oil / fat composition is 100% by mass by calculating the determination value of the determination target oil / fat composition and comparing it with the 100% mass determination value. The method for judging an oil or fat composition according to the above [1], wherein the oil composition is judged.
[6] A first fluorescent fingerprint obtained by exciting oil A with a spectrofluorometer at all or part of the excitation wavelength of 250 to 700 nm and measuring all or part of the fluorescence wavelength of 250 to 800 nm. And the second fluorescent fingerprint of the determination target oil / fat composition obtained by measuring under the same conditions as the measurement conditions of the first fluorescent fingerprint, whereby the oil / fat composition is composed only of the oil / fat A. The determination method of the oil-fat composition which determines whether or not.
[7] The method for judging an oil composition according to [6], wherein the fat A is a refined vegetable oil.
[8] Oil and fat A and fat B are added so as to have a desired content ratio, mixed by a mixing device to obtain an oil and fat composition, and 1 characteristic of the oil and fat A and / or the oil and fat B The determination step of determining the content ratio of the fat A and the fat B in the fat composition by measuring the fluorescence intensity of one or more peaks, and the determined content ratio deviates from the desired content ratio. In the mixing step, in the mixing step, an adjustment step of increasing the addition amount of the fat that is less than the desired content ratio and / or reducing the addition amount of the fat that exceeds the desired content proportion The manufacturing method of the oil-fat composition characterized by having.
[9] The fat / oil in the fat / oil composition using the mixing step of adding the fat / oil A and the fat / oil B to a desired content ratio and mixing with a mixing device to obtain the fat / oil composition, and the following determination method A determination step of determining a content ratio of A and the fats and oils B, and a case where the determined content ratio is out of the desired content ratio, the mixing step is less than the desired content ratio The manufacturing method of the oil-fat composition characterized by having the adjustment process which increases the addition amount of fats and oils and / or reduces the addition amount of the fats and oils which exceed the said desired content rate. Judgment method: Two or more selected from fat and oil composition containing fat and oil A, fat and oil B, and the fat and oil A and the fat and oil B, using a spectrofluorimeter, all or part of the excitation wavelength of 250 to 700 nm. One or more peaks characteristic of the fats and oils A and / or the fats and oils B are selected by comparing each fluorescent fingerprint obtained by exciting and measuring all or part of the fluorescence wavelength of 250 to 800 nm, By measuring the fluorescence intensity of the oil composition to be determined at one or more wavelengths of the peak (excitation wavelength, fluorescence wavelength) using a fluorometer, the fat A and oil A in the oil composition to be determined and / Or the content ratio of the said fats and oils B is determined.
[10] Fluorescence intensity of the fat composition in which the content ratio of the fat A and the fat B is known at one or more of the peak wavelengths (excitation wavelength, fluorescence wavelength) using a spectrofluorometer A calibration curve is created with the fluorescence intensity as the horizontal axis or the vertical axis, and the concentration of the fat or oil A as the vertical axis or the horizontal axis, and the fluorescence intensity of the determination target oil or fat composition is compared with the calibration curve. By performing, the content ratio of the said fats and oils A and the said fats and oils B in the said fats and oils composition of the determination object is determined, The manufacturing method of the oil and fat composition as described in said [9] characterized by the above-mentioned.
[11] The method for producing an oil / fat composition according to any one of [8] to [10], wherein the mixing device is an in-line mixing device or a batch-type mixing device.
本発明によると、油脂組成物中の油脂の含量比を精度良く判定できる油脂組成物の判定方法及び所望の含量比の油脂組成物を製造できる油脂組成物の製造方法を提供することができる。本発明によると、ガスクロマトグラフィーを使用する場合に比べて油脂組成物中の油脂の含量比を短時間で判定できる油脂組成物の判定方法及び所望の含量比の油脂組成物を効率よく製造できる油脂組成物の製造方法を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the determination method of the oil-fat composition which can determine the content ratio of fats and oils in an oil-fat composition accurately, and the manufacturing method of the oil-fat composition which can manufacture the oil-fat composition of desired content ratio can be provided. According to the present invention, it is possible to efficiently produce an oil / fat composition having a desired content ratio and a method for determining an oil / fat composition capable of determining the content ratio of the oil / fat in the oil / fat composition in a short time compared to the case of using gas chromatography. The manufacturing method of an oil-fat composition can be provided.
また、本発明によると、他の油脂の混入率が低い場合や双方の油脂の脂肪酸組成が類似している場合であっても１００％純正の油脂であるか否かや偽造品であるか否かの正確な判定ができる油脂組成物の判定方法を提供することができる。 Further, according to the present invention, even if the mixing rate of other fats and oils is low or the fatty acid compositions of both fats and oils are similar, whether or not they are 100% genuine fats or oils or counterfeits. It is possible to provide a method for determining an oil / fat composition capable of accurately determining the above.
〔油脂組成物の判定方法〕
本発明の実施形態に係る油脂組成物の判定方法は、油脂Ａ、油脂Ｂ、及び前記油脂Ａと前記油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた各蛍光指紋を比較して前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で判定対象の油脂組成物の蛍光強度を測定することにより、前記判定対象の油脂組成物中の前記油脂Ａ及び／又は前記油脂Ｂの含量割合を判定する。
[Determination method of oil and fat composition]
The determination method of the oil-fat composition which concerns on embodiment of this invention uses two or more chosen from fats and oils composition containing fats and oils A, fats and oils B, and the said fats and oils A and the said fats and oils B using a spectrofluorimeter. The fats and oils B and / or the fats and oils B are characterized by comparing fluorescent fingerprints obtained by exciting all or part of the excitation wavelengths of 250 to 700 nm and measuring all or part of the fluorescence wavelengths of 250 to 800 nm. By selecting one or more specific peaks and measuring the fluorescence intensity of the oil composition to be judged at the wavelength of the one or more peaks (excitation wavelength, fluorescence wavelength) using a spectrofluorometer, The content ratio of the fat / oil A and / or the fat / oil B in the fat / oil composition to be determined is determined.
本実施の形態における判定方法においては、判定対象の油脂組成物中に含有されている油脂が油脂Ａ及び／又は油脂Ｂであると分かっている（既知である）ことが前提である。なお、必ずしも油脂Ａや油脂Ｂの原料や産地等まで既知でなくてもよく、同じ物が入手できる程度に特定できていればよい。 In the determination method in the present embodiment, it is premised that the fats and oils contained in the judgment target oil and fat composition are known to be fats and oils A and / or fats and oils B (known). In addition, it does not necessarily need to be known to the raw material, production center, etc. of fats and oils A and fats B, and it should just be specified to such an extent that the same thing can be obtained.
（蛍光指紋の測定）
初めに、油脂Ａ、油脂Ｂ、及び油脂Ａと油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍ全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して各蛍光指紋を得る。
(Measurement of fluorescent fingerprint)
First, two or more selected from fat and oil composition containing fat and oil A, fat and oil B, and fat and oil A and fat and oil B are excited using a spectrofluorimeter at all or part of an excitation wavelength of 250 to 700 nm. Each fluorescence fingerprint is obtained by measuring all or part of the fluorescence wavelength of 250 to 800 nm.
測定対象としては、油脂Ａ（１００質量％）、油脂Ｂ（１００質量％）、及び油脂Ａと油脂Ｂとを含む油脂組成物から選ばれるいずれか２つ以上であるが、３つすべてを測定対象とすることが好ましい。また、油脂Ａと油脂Ｂとを含む油脂組成物は、種々の含量比のものを測定対象とすることが好ましい。例えば、油脂Ａと油脂Ｂの含量比（質量）が、油脂Ａ：油脂Ｂ＝９９：１、９５：５、９０：１０、７５：２５、５０：５０、２５：７５、１０：９０、５：９５、１：９９のものを測定対象とする。 As a measuring object, it is any two or more chosen from fats and oils composition containing fats and oils A (100 mass%), fats and oils B (100 mass%), and fats and oils A and fats and oils B, but all three are measured. It is preferable to make it a target. Moreover, it is preferable that the fats and oils composition containing the fats and oils A and the fats and oils B make a measurement object the thing of various content ratio. For example, the content ratio (mass) of fat / oil A and fat / oil B is fat / oil A: fat / oil B = 99: 1, 95: 5, 90:10, 75:25, 50:50, 25:75, 10:90, 5 : 95, 1:99
油脂Ａ及び油脂Ｂとしては、特に限定されることなく、種々の油脂に適用できる。例えば、好適な一実施形態では、油脂Ａが未精製植物油であり、油脂Ｂが精製植物油である。また、好適な別の一実施形態では、油脂Ａ及び油脂Ｂが、精製植物油である。 The fats and oils A and B are not particularly limited and can be applied to various fats and oils. For example, in one suitable embodiment, fats and oils A are unrefined vegetable oils, and fats and oils B are refined vegetable oils. Moreover, in another suitable embodiment, fats and oils A and fats and oils B are refined vegetable oils.
本発明の実施形態に適用可能な植物油としては、例えば、大豆油、菜種油、高オレイン酸菜種油、オリーブ油、コーン油、ゴマ油、シソ油、亜麻仁油、落花生油、紅花油、高オレイン酸紅花油、ひまわり油、高オレイン酸ひまわり油、綿実油、ブドウ種子油、マカデミアナッツ油、ヘーゼルナッツ油、カボチャ種子油、クルミ油、椿油、茶実油、エゴマ油、ボラージ油、米油、小麦胚芽油、パーム油、パーム核油、ヤシ油、カカオ脂、品種改良によって低飽和化されたこれらの油脂等が挙げられる。植物油以外では、牛脂、ラード、鶏脂、乳脂、魚油、アザラシ油、藻類油等が挙げられる。 Examples of vegetable oils that can be applied to the embodiments of the present invention include soybean oil, rapeseed oil, high oleic rapeseed oil, olive oil, corn oil, sesame oil, perilla oil, linseed oil, peanut oil, safflower oil, and high oleic safflower oil. Sunflower oil, high oleic sunflower oil, cottonseed oil, grape seed oil, macadamia nut oil, hazelnut oil, pumpkin seed oil, walnut oil, coconut oil, tea seed oil, sesame oil, borage oil, rice oil, wheat germ oil, palm oil, Examples thereof include palm kernel oil, coconut oil, cacao butter, and these oils and fats that have been low-saturated by variety improvement. Other than vegetable oils, beef tallow, lard, chicken fat, milk fat, fish oil, seal oil, algal oil and the like.
使用する分光蛍光光度計は、高精度かつ高速に測定を行なうことができる装置であることが望ましく、例えば、株式会社日立ハイテクサイエンス製のＦ−７０００形やＦ−７１００形が好適に使用できる。 The spectrofluorometer to be used is desirably a device capable of performing high-precision and high-speed measurement. For example, F-7000 type or F-7100 type manufactured by Hitachi High-Tech Science Co., Ltd. can be suitably used.
分光蛍光光度計による測定においては、測定対象の油脂又は油脂組成物を励起波長２５０〜７００ｎｍ全部あるいは一部の光（励起光）で励起させる。そして、蛍光波長２５０〜７００ｎｍの全部あるいは一部を測定する。一部とは、例えば、励起波長３００〜４５０ｎｍで蛍光波長６４５〜７００ｎｍ、あるいは、励起波長３４０〜４００ｎｍで蛍光波長３６０〜５６０ｎｍ、励起波長２８５〜３２０ｎｍで蛍光波長３７０〜５３０ｎｍを含むものである。 In the measurement with a spectrofluorometer, the oil or fat composition to be measured is excited with all or part of the excitation wavelength of 250 to 700 nm (excitation light). Then, all or a part of the fluorescence wavelength of 250 to 700 nm is measured. The part includes, for example, a fluorescence wavelength of 645 to 700 nm at an excitation wavelength of 300 to 450 nm, a fluorescence wavelength of 360 to 560 nm at an excitation wavelength of 340 to 400 nm, and a fluorescence wavelength of 370 to 530 nm at an excitation wavelength of 285 to 320 nm.
（特徴的なピークの選択）
次に、得られた蛍光指紋を比較して油脂Ａ及び／又は油脂Ｂに特徴的な１個以上のピークを選択する。油脂Ａ及び油脂Ｂに特徴的な１個以上のピークをそれぞれ選択することが好ましい。選択方法としては、例えば、油脂Ａと油脂Ｂを含有する油脂組成物において油脂Ａの含有量が増えるほどより顕著に現れるピークを油脂Ａに特徴的なピークとして選択し、油脂Ｂの含有量が増えるほどより顕著に現れるピークを油脂Ｂに特徴的なピークとして選択する。
油脂Ａ又は油脂Ｂに特徴的な１種のピークが分かれば、そのピークの蛍光強度から油脂Ａと油脂Ｂの各含量割合が分かる。
(Selecting characteristic peaks)
Next, the obtained fluorescent fingerprints are compared, and one or more peaks characteristic to the fat A and / or the fat B are selected. It is preferable to select one or more peaks characteristic of the fat A and the fat B, respectively. As a selection method, for example, a peak that appears more prominently as the content of fat or oil A increases in the fat or oil composition containing fat or oil A and fat B is selected as a characteristic peak for fat or oil A, and the content of fat or oil B is The peak that appears more prominently as it increases is selected as a characteristic peak for the fat B.
If one kind of peak characteristic to fats and oils A or fats and oils B is known, each content ratio of fats and oils A and fats and oils B can be known from the fluorescence intensity of the peaks.
（蛍光強度の測定）
次に、分光蛍光光度計を用いて、選択した１個以上のピークの波長（励起波長、蛍光波長）で判定対象の油脂組成物の蛍光強度を測定する。この時用いる分光蛍光光度計は、測定対象の波長が測定できるものであればよく、単波長、又は複数波長を測定する分光蛍光光度計、あるいは前述の蛍光指紋の測定で用いた分光蛍光光度計等を用いることができる。
(Measurement of fluorescence intensity)
Next, using a spectrofluorometer, the fluorescence intensity of the determination target oil or fat composition is measured at one or more selected peak wavelengths (excitation wavelength, fluorescence wavelength). The spectrofluorimeter used at this time is not limited as long as it can measure the wavelength of the object to be measured. The spectrofluorometer that measures a single wavelength or a plurality of wavelengths, or the spectrofluorometer used in the measurement of the fluorescence fingerprint described above. Etc. can be used.
（含量比の判定）
測定して得られた蛍光強度を用いることにより、判定対象の油脂組成物中の油脂Ａ及び／又は油脂Ｂの含量割合を判定することができる。
(Determination of content ratio)
By using the fluorescence intensity obtained by measurement, the content ratio of the fat A and / or the fat B in the determination target oil composition can be determined.
例えば、本発明の一実施形態においては、分光蛍光光度計を用いて、選択した１個以上のピークの波長（励起波長、蛍光波長）で油脂Ａと油脂Ｂの含量割合が既知の油脂組成物の蛍光強度を測定し、当該蛍光強度を横軸とし、油脂Ａの濃度を縦軸として検量線を作成しておき、判定対象の油脂組成物の蛍光強度を当該検量線と比較することにより、判定対象の油脂組成物中の油脂Ａ及び／又は油脂Ｂの含量割合を判定することができる。横軸と縦軸とを逆にした検量線でもよい。 For example, in one embodiment of the present invention, an oil / fat composition having a known content ratio of oil / fat A / fat B at a wavelength of one or more selected peaks (excitation wavelength, fluorescence wavelength) using a spectrofluorometer. By measuring the fluorescence intensity of the sample, preparing a calibration curve with the fluorescence intensity as the horizontal axis and the fat and oil A concentration as the vertical axis, and comparing the fluorescence intensity of the determination target oil composition with the calibration curve, The content ratio of fats and oils A and / or fats and oils B in the oil and fat composition to be judged can be judged. A calibration curve with the horizontal and vertical axes reversed may be used.
（含量１００質量％であるか否かの判定）
また、本発明の実施形態に係る油脂組成物の判定方法の別の一実施形態においては、上記の得られた各蛍光指紋を比較して油脂Ａに特徴的な１個以上のピーク及び油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて油脂Ａに特徴的な１個以上のピークの波長（励起波長、蛍光波長）のうちの１以上で油脂Ａと油脂Ｂの含量比が既知の油脂組成物の蛍光強度Ａを測定し、かつ油脂Ｂに特徴的な１個以上のピークの波長（励起波長、蛍光波長）のうちの１以上で油脂Ａと油脂Ｂの含量割合が既知の油脂組成物の蛍光強度Ｂを測定し、「蛍光強度Ａの合計値／蛍光強度Ｂの合計値」の比率又は「蛍光強度Ｂの合計値／蛍光強度Ａの合計値」の比率を判定値として算出して検量線を作成し、油脂Ａの含量比が１００質量％であると判定できる１００質量％判定値を求め、判定対象の油脂組成物の上記判定値を算出して上記１００質量％判定値と比較することにより、判定対象の油脂組成物中の油脂Ａの含量が１００質量％であるか否かを判定する。
(Determination of whether the content is 100% by mass)
Moreover, in another one Embodiment of the determination method of the oil-fat composition which concerns on embodiment of this invention, one or more peaks and oil-fat B which are characteristic of the oil-fat A by comparing each said fluorescence fingerprint obtained above. One or more peaks characteristic of the oil and fat are selected and one or more of the wavelengths (excitation wavelength, fluorescence wavelength) of the one or more peaks characteristic of the fat and oil A are measured using a spectrofluorophotometer. Measure the fluorescence intensity A of an oil / fat composition whose B content ratio is known, and the oil / fat A and the oil / fat B at one or more of one or more peak wavelengths (excitation wavelength, fluorescence wavelength) characteristic of the oil / fat B The fluorescence intensity B of the oil / fat composition with a known content ratio is measured, and the ratio of “total value of fluorescence intensity A / total value of fluorescence intensity B” or “total value of fluorescence intensity B / total value of fluorescence intensity A” A calibration curve is created by calculating the ratio of the above as a judgment value, and the content ratio of fat A is 100% by mass 100% by mass determination value that can be determined, the above determination value of the determination target oil composition is calculated and compared with the above 100% by mass determination value, whereby the content of the fat A in the determination target oil composition is 100 It is determined whether it is mass%.
詳細な具体例については、後述する実施例にて説明するが、本実施形態によれば、他の油脂の混入率が低い場合や双方の油脂の脂肪酸組成が類似している場合であっても１００％純正の油脂であるか否かや偽造品であるか否かの正確な判定をすることができる。 Although a specific example is demonstrated in the Example mentioned later, even if it is a case where the fatty acid composition of both fats and oils is similar according to this embodiment, when the mixing rate of other fats and oils is low. It is possible to accurately determine whether the oil is 100% genuine oil or not and whether it is a counterfeit product.
また、本発明の実施形態に係る油脂組成物の判定方法の別の一実施形態においては、油脂Ａを、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた第１の蛍光指紋と、第１の蛍光指紋の測定条件と同条件で測定して得られる判定対象の油脂組成物の第２の蛍光指紋とを比較することにより、判定対象の油脂組成物が油脂Ａのみからなるか否かを判定することができる。 In another embodiment of the method for determining an oil composition according to an embodiment of the present invention, the oil A is excited with all or part of an excitation wavelength of 250 to 700 nm using a spectrofluorimeter. A first fluorescent fingerprint obtained by measuring all or part of the fluorescence wavelength of 250 to 800 nm, and a second determination target oil / fat composition obtained by measurement under the same measurement conditions as the first fluorescent fingerprint. It is possible to determine whether or not the oil / fat composition to be determined consists only of the oil / fat A by comparing the fluorescent fingerprint of
本実施形態における適用可能な油脂Ａ、使用する分光蛍光光度計、及び分光蛍光光度計による蛍光指紋の測定条件は、前述の実施形態と同様である。 The applicable conditions for the oil and fat A, the spectrofluorometer to be used, and the fluorescence fingerprint measurement conditions using the spectrofluorometer in the present embodiment are the same as those in the previous embodiment.
第１の蛍光指紋と第２の蛍光指紋とを比較した結果、同一の蛍光指紋であれば、判定対象の油脂組成物が油脂Ａのみからなると言える。 As a result of comparing the first fluorescent fingerprint and the second fluorescent fingerprint, if the same fluorescent fingerprint is used, it can be said that the oil / fat composition to be determined consists only of the oil / fat A.
〔油脂組成物の製造方法〕
本発明の実施形態に係る油脂組成物の製造方法の一実施形態は、油脂Ａと油脂Ｂとを所望の含量割合で含有する油脂組成物の製造方法であって、油脂Ａと油脂Ｂとを所望の含量割合となるように添加し、インライン式混合装置又はバッチ式混合装置により混合して油脂組成物を得る混合工程と、油脂Ａ及び／又は油脂Ｂに特徴的なピークの蛍光強度を測定することにより、前記油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定する判定工程と、前記判定された含量割合が前記所望の含量割合を外れている場合に、前記混合工程において、前記所望の含量割合を下回っている方の油脂の添加量を増やす、及び／又は前記所望の含量割合を超えている方の油脂の添加量を減らす調整工程を有する。以下、これらの工程を順に説明する。
[Method for producing oil and fat composition]
One embodiment of a method for producing an oil / fat composition according to an embodiment of the present invention is a method for producing an oil / fat composition containing oil / fat A and oil / fat B in a desired content ratio. Add to desired content ratio, mix with in-line mixing device or batch mixing device to obtain oil composition, and measure fluorescence intensity of peak characteristic of oil A and / or oil B In the mixing step, when the determination step of determining the content ratio of the fat A and the fat B in the fat composition, and the determined content ratio deviates from the desired content ratio And an adjustment step of increasing the amount of the fat that is less than the desired content ratio and / or decreasing the amount of the fat that exceeds the desired content ratio. Hereinafter, these steps will be described in order.
（混合工程）
混合工程においては、油脂Ａと油脂Ｂとを所望の含量割合となるように添加しインライン式混合装置又はバッチ式混合装置により混合して油脂組成物を得る。
(Mixing process)
In a mixing process, fats and oils A and fats and oils B are added so that it may become a desired content ratio, and it mixes with an in-line type mixing apparatus or a batch type mixing apparatus, and obtains an oil and fat composition.
図１１は、本発明の実施の形態に係る油脂組成物の製造方法におけるインライン式混合装置１０を示す概略図である。
油脂Ａ（符号１、以下省略）は油導入管１１の流入口１１Ａから供給され、油脂Ｂ（符号２、以下省略）は流入口１１Ｂから供給される。油脂Ａ及び油脂Ｂの供給量は、流入口１１Ａ及び流入口１１Ｂに設けられたバルブ（図示省略）により流速（流量）制御がなされている。油導入管１１に供給された油脂Ａ及び油脂Ｂは、スタティックミキサー１２を通過する際に混合されて混合油Ｃ（符号３、以下省略）となり、油送管１３へ流れていく。本実施形態においてはスタティックミキサーを用いたが、インラインで設置できるものであればよく、混合機はこれに限られない。
FIG. 11 is a schematic view showing an in-line mixing device 10 in the method for producing an oil and fat composition according to the embodiment of the present invention.
Oil A (reference numeral 1, omitted hereinafter) is supplied from the inlet 11A of the oil introduction pipe 11, and oil B (reference numeral 2, omitted below) is supplied from the inlet 11B. The supply amount of the fats and oils A and fats and oils B is controlled in flow velocity (flow rate) by valves (not shown) provided at the inlet 11A and the inlet 11B. The fats A and B supplied to the oil introduction pipe 11 are mixed when passing through the static mixer 12 to become a mixed oil C (reference numeral 3, hereinafter omitted) and flow to the oil feed pipe 13. Although a static mixer is used in the present embodiment, any mixer that can be installed in-line may be used, and the mixer is not limited to this.
図１２は、本発明の実施の形態に係る油脂組成物の製造方法におけるバッチ式混合装置２０を示す概略図である。
油脂Ａ及び油脂Ｂは、撹拌槽２１に供給され、モーター２３を備えた攪拌機２２により撹拌混合されて混合油Ｃとなる。油脂Ａ及び油脂Ｂの供給量は、図示を省略したバルブにより流速（流量）制御がなされている。
FIG. 12 is a schematic view showing a batch type mixing apparatus 20 in the method for producing an oil and fat composition according to the embodiment of the present invention.
The fats and oils A and fats and oils B are supplied to the stirring tank 21, and are stirred and mixed by a stirrer 22 equipped with a motor 23 to become a mixed oil C. The supply amount of the fats and oils A and the fats and oils B is controlled in flow rate (flow rate) by a valve not shown.
（判定工程）
判定工程においては、前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークの蛍光強度を測定することにより、油脂組成物（混合油Ｃ）中の油脂Ａと油脂Ｂの含量比を判定する。なお、前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークは、前記油脂Ａ、前記油脂Ｂ、及び前記油脂Ａと前記油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた各蛍光指紋を比較して選択する。詳細は上記本発明の実施形態に係る油脂組成物の判定方法に記載の通りである。
蛍光指紋や蛍光強度の測定は、図１１のインライン式混合装置１０では、油送管１３に設置された分光蛍光光度計１４により行なう。インラインでの設置が困難な場合には、油送管１３に混合油Ｃの採取口を設け、混合油Ｃを採取し、外部の分光蛍光光度計により測定することとしてもよい。
なお、使用する分光蛍光光度計は、測定するピークが検出可能な範囲のものでよく、前述の蛍光指紋を測定できる分光蛍光光度計の他、単波長のみの蛍光波長を測定する分光蛍光光度計も使用できる。
一方、図１２のバッチ式混合装置２０では、蛍光指紋や蛍光強度の測定は、撹拌槽２１内部又は外部に設置した分光蛍光光度計（図示省略）により行なう。
(Judgment process)
In the determination step, the content ratio of fat A and fat B in the fat composition (mixed oil C) is measured by measuring the fluorescence intensity of one or more peaks characteristic of the fat A and / or fat B. Determine. In addition, the one or more peaks characteristic of the oil and fat A and / or the oil and fat B are two or more selected from the oil and fat composition including the oil and fat A, the oil and fat B, and the oil and fat A and the oil and fat B. Using a spectrofluorometer, the excitation wavelength is excited at all or part of 250 to 700 nm, and the fluorescence fingerprints obtained by measuring all or part of the fluorescence wavelength of 250 to 800 nm are compared and selected. . The details are as described in the determination method of the oil and fat composition according to the embodiment of the present invention.
The fluorescence fingerprint and the fluorescence intensity are measured by the spectrofluorometer 14 installed in the oil feed pipe 13 in the in-line type mixing apparatus 10 of FIG. If installation in-line is difficult, the oil feed pipe 13 may be provided with a sampling port for the mixed oil C, and the mixed oil C may be sampled and measured with an external spectrofluorometer.
The spectrofluorometer used may be in a range where the peak to be measured can be detected. In addition to the spectrofluorometer capable of measuring the fluorescent fingerprint described above, the spectrofluorometer that measures only a single wavelength of fluorescence. Can also be used.
On the other hand, in the batch type mixing apparatus 20 of FIG. 12, the fluorescence fingerprint and the fluorescence intensity are measured by a spectrofluorometer (not shown) installed inside or outside the stirring tank 21.
（調整工程）
調整工程においては、上記判定工程で判定された含量比が所望の含量比を外れている場合に、上記混合工程において、所望の含量割合を下回っている方の油脂の添加量を増やす（流速をアップする）、及び／又は所望の含量比を超えている方の油脂の添加量を減らす（流速をダウンする）ことにより調整を行なう。
(Adjustment process)
In the adjustment step, when the content ratio determined in the determination step is out of the desired content ratio, in the mixing step, the amount of oil or fat that is less than the desired content ratio is increased (flow rate is increased). Up) and / or by adjusting the amount of fat or oil that exceeds the desired content ratio (decreasing the flow rate).
次に実施例により本発明を説明するが、本発明はこれらの実施例により限定されるものではない。 EXAMPLES Next, although an Example demonstrates this invention, this invention is not limited by these Examples.
〔実施例１〕
（蛍光指紋の測定）
エキストラバージンオリーブオイル（ＥＶＯＯ）（日清オイリオグループ株式会社製、スペイン産）及び／又は精製オリーブオイル（ＲＯＯ）（日清オイリオグループ株式会社製）からなる油脂組成物の蛍光指紋を分光蛍光光度計（商品名：Ｆ−７０００、株式会社日立ハイテクサイエンス社製）により測定した。測定結果を図１に示す。
[Example 1]
(Measurement of fluorescent fingerprint)
Fluorescent fingerprint of oil composition comprising extra virgin olive oil (EVOO) (Nisshin Oillio Group Co., Ltd., Spain) and / or refined olive oil (ROO) (Nisshin Oillio Group Co., Ltd.) (Product name: F-7000, manufactured by Hitachi High-Tech Science Co., Ltd.). The measurement results are shown in FIG.
図１は、種々の含量比のエキストラバージンオリーブオイル（ＥＶＯＯ）と精製オリーブオイル（ＲＯＯ）とからなる油脂組成物の蛍光指紋である。各図の油脂組成物の含量比（ＥＶＯＯ：ＲＯＯ）は、（ａ）は１００：０、（ｂ）は９９：１、（ｃ）は９７．５：２．５、（ｄ）は９５：５、（ｅ）は９０：１０、（ｆ）は７５：２５、（ｇ）は５０：５０、（ｈ）は２５：７５、（ｉ）は１０：９０、（ｊ）は５：９５、（ｋ）は０：１００である。 FIG. 1 is a fluorescent fingerprint of an oil / fat composition comprising extra virgin olive oil (EVOO) and refined olive oil (ROO) in various content ratios. The oil / fat composition ratio (EVOO: ROO) in each figure is (a) 100: 0, (b) 99: 1, (c) 97.5: 2.5, (d) 95: 5, (e) is 90:10, (f) is 75:25, (g) is 50:50, (h) is 25:75, (i) is 10:90, (j) is 5:95, (K) is 0: 100.
また、各油脂組成物について２５℃における屈折率（ＲＩ）を屈折計（京都電子工業株式会社製）により測定した結果も図１に示す。 Moreover, the result of having measured the refractive index (RI) in 25 degreeC about each oil-fat composition with the refractometer (made by Kyoto Electronics Industry Co., Ltd.) is also shown in FIG.
（特徴的なピークの選択）
得られた蛍光指紋を比較してＥＶＯＯ及び／又はＲＯＯに特徴的な１０個のピークを選択した。なお、特徴的なピークは、目視にて判別したが、多変量解析ソフトウェア等を用いて行ってもよい。
(Selecting characteristic peaks)
Ten peaks characteristic of EVOO and / or ROO were selected by comparing the obtained fluorescent fingerprints. In addition, although the characteristic peak was discriminate | determined visually, you may carry out using multivariate analysis software etc.
図２（ａ）は図１（ｇ）の蛍光指紋において選択した１０個のピークの位置を示す図であり、図２（ｂ）は図２（ａ）に示す１０個のピークにおける励起波長（ＥＸ）と蛍光波長（ＥＭ）である。 FIG. 2A is a diagram showing the positions of 10 peaks selected in the fluorescent fingerprint of FIG. 1G, and FIG. 2B is an excitation wavelength (10) at the 10 peaks shown in FIG. EX) and fluorescence wavelength (EM).
各蛍光指紋の比較により、Ｎｏ．２〜４がＲＯＯに特徴的なピーク、Ｎｏ．５〜１０がＥＶＯＯに特徴的なピークであると考察した。 From comparison of each fluorescent fingerprint, no. Nos. 2 to 4 are peaks characteristic of ROO. 5-10 were considered to be characteristic peaks for EVOO.
（蛍光強度の測定）
上記分光蛍光光度計を用いて、１０個のピークの波長（励起波長、蛍光波長）でＥＶＯＯとＲＯＯの含量比が既知の油脂組成物の蛍光強度を測定した。測定した油脂組成物は１１種であり、その含量比は、ＥＶＯＯ：ＲＯＯ＝１００：０、９９：１、９７．５：２．５、９５：５、９０：１０、７５：２５、５０：５０、２５：７５、１０：９０、５：９５、０：１００である。なお、蛍光強度は、硫酸キニーネ補正をかけて求めた（以下、同様）。
(Measurement of fluorescence intensity)
Using the above spectrofluorometer, the fluorescence intensity of an oil / fat composition having a known content ratio of EVOO and ROO was measured at 10 peak wavelengths (excitation wavelength, fluorescence wavelength). The measured fat and oil composition was 11 kinds, and the content ratio was EVOO: ROO = 100: 0, 99: 1, 97.5: 2.5, 95: 5, 90:10, 75:25, 50: 50, 25:75, 10:90, 5:95, 0: 100. The fluorescence intensity was determined by correcting for quinine sulfate (hereinafter the same).
１０個のピークのうちのＮｏ．１を除くＮｏ．２〜１０の９個のピークについて、測定した蛍光強度を横軸とし、ＥＶＯＯの濃度を縦軸として検量線を作成した。決定係数（Ｒ２）はいずれも０．９以上となり、非常に良好な検量線を得ることができた。 No. of 10 peaks. No. 1 Calibration curves were prepared for 9 peaks from 2 to 10 with the measured fluorescence intensity as the horizontal axis and the EVOO concentration as the vertical axis. The determination coefficient (R 2 ) was 0.9 or more in all cases, and a very good calibration curve could be obtained.
Ｎｏ．１の励起波長（ＥＸ）３００ｎｍ、蛍光波長（ＥＭ）３２５ｎｍについては、ＥＶＯＯ濃度やＲＯＯ濃度に依存せずに一定の蛍光強度を得られた。よって、油脂固有の蛍光強度と考え、検量線を描かなかった。 No. With an excitation wavelength (EX) of 300 nm and a fluorescence wavelength (EM) of 325 nm, a constant fluorescence intensity was obtained without depending on the EVOO concentration or the ROO concentration. Therefore, a calibration curve was not drawn considering that the fluorescence intensity was unique to the oil.
図３は、図２（ａ）に示すＮｏ．２〜１０のピークにおける励起波長（ＥＸ）と蛍光波長（ＥＭ）で測定した蛍光強度（横軸）とＥＶＯＯ濃度（縦軸）との関係を示す検量線である。（ａ）〜（ｉ）は、順にＮｏ．２〜１０のピークにおける検量線である。 FIG. 3 shows No. 1 shown in FIG. It is a calibration curve which shows the relationship between the fluorescence intensity (horizontal axis) and the EVOO concentration (vertical axis) measured by the excitation wavelength (EX) and the fluorescence wavelength (EM) at 2-10 peaks. (A)-(i) are No. in order. It is a calibration curve at 2-10 peaks.
上記分光蛍光光度計を用いて、選択した１０個のうちのＮｏ．１を除くＮｏ．２〜９の９個のピークの波長（励起波長、蛍光波長）のいずれか１以上で判定対象の油脂組成物の蛍光強度を測定する。 Using the above spectrofluorometer, No. 10 out of 10 selected. No. 1 The fluorescence intensity of the oil / fat composition to be determined is measured at any one or more of 9 peak wavelengths (excitation wavelength, fluorescence wavelength) of 2 to 9.
（含量比の判定）
測定して得られる判定対象の油脂組成物の蛍光強度を上記検量線と比較することにより、判定対象の油脂組成物中の油脂Ａと油脂Ｂの含量比を判定することができる。
(Determination of content ratio)
By comparing the fluorescence intensity of the determination target oil composition obtained by measurement with the calibration curve, the content ratio of the fat A and the fat B in the determination target oil composition can be determined.
（含量１００質量％であるか否かの判定）
次に、油脂組成物中のＥＶＯＯの含量が１００質量％であるか否かを以下の方法により判定した。
(Determination of whether the content is 100% by mass)
Next, whether or not the content of EVOO in the oil and fat composition was 100% by mass was determined by the following method.
図１の各蛍光指紋を比較してＲＯＯに特徴的な３個のピーク（Ｎｏ．２〜４）及びＥＶＯＯに特徴的な６個のピーク（Ｎｏ．５〜１０）を選択した。 Each fluorescent fingerprint of FIG. 1 was compared, and three peaks (No. 2 to 4) characteristic for ROO and six peaks (No. 5 to 10) characteristic for EVOO were selected.
前述の分光蛍光光度計を用いてＲＯＯに特徴的な３個のピーク（Ｎｏ．２〜４）の波長（励起波長、蛍光波長）のうちの１以上でＥＶＯＯとＲＯＯの含量比が既知の油脂組成物の蛍光強度Ａを測定し、かつＥＶＯＯに特徴的な６個のピーク（Ｎｏ．５〜１０）の波長（励起波長、蛍光波長）のうちの１以上でＥＶＯＯとＲＯＯの含量比が既知の油脂組成物の蛍光強度Ｂを測定した。測定データは、図３の検量線の作成に用いた蛍光強度のデータを使用した。 Fats and oils whose content ratio of EVOO and ROO is known at one or more of the wavelengths (excitation wavelength, fluorescence wavelength) of the three peaks (No. 2 to 4) characteristic of ROO using the spectrofluorometer described above The fluorescence intensity A of the composition is measured, and the content ratio of EVOO and ROO is known at one or more of the wavelengths (excitation wavelength, fluorescence wavelength) of the six peaks (No. 5 to 10) characteristic of EVOO The fluorescence intensity B of the oil and fat composition was measured. As the measurement data, the fluorescence intensity data used to create the calibration curve of FIG. 3 was used.
「蛍光強度Ｂの合計値／蛍光強度Ａの合計値」（判別式）で算出した値を判定値として検量線を作成した。なお、「蛍光強度Ａの合計値／蛍光強度Ｂの合計値」（判別式）を算出して判定値とすることもできる。 A calibration curve was created using the value calculated by “total value of fluorescence intensity B / total value of fluorescence intensity A” (discriminant) as a determination value. It should be noted that “the total value of the fluorescence intensity A / the total value of the fluorescence intensity B” (discriminant) may be calculated and used as the determination value.
ＥＶＯＯにおいてＮｏ．４（ＥＸ３６０，ＥＭ４００）はほとんど出ない蛍光強度であり、ＲＯＯ（精製植物油）では検出される特徴的な蛍光強度であった。そこで、その点を考慮した判別式１〜４を作成した。 No. in EVOO 4 (EX360, EM400) was a fluorescence intensity that hardly appeared, and was a characteristic fluorescence intensity detected by ROO (refined vegetable oil). Therefore, discriminants 1 to 4 were created in consideration of this point.
判別式１：Ｎｏ．５〜１０の波長で測定した蛍光強度Ｂの合計値／Ｎｏ．４の波長で測定した蛍光強度Ａの合計値
判別式２：Ｎｏ．５〜１０の波長で測定した蛍光強度Ｂの合計値／Ｎｏ．３〜４の波長で測定した蛍光強度Ａの合計値
判別式３：Ｎｏ．５〜１０の波長で測定した蛍光強度Ｂの合計値／Ｎｏ．２及び４の波長で測定した蛍光強度Ａの合計値
判別式４：Ｎｏ．５〜１０の波長で測定した蛍光強度Ｂの合計値／Ｎｏ．２〜４の波長で測定した蛍光強度Ａの合計値
Discriminant 1: No. Total value of fluorescence intensity B measured at wavelengths of 5 to 10 / No. Total value of fluorescence intensity A measured at the wavelength of 4 Discriminant 2: No. Total value of fluorescence intensity B measured at wavelengths of 5 to 10 / No. Total value of fluorescence intensity A measured at wavelengths 3-4 Discriminant 3: No. Total value of fluorescence intensity B measured at wavelengths of 5 to 10 / No. Total value of fluorescence intensity A measured at wavelengths 2 and 4 Discriminant 4: No. Total value of fluorescence intensity B measured at wavelengths of 5 to 10 / No. Total value of fluorescence intensity A measured at wavelengths of 2-4
図４〜７は、それぞれ判別式１〜４で算出した判定値（横軸）とＥＶＯＯ濃度（縦軸）との関係を示す検量線である。決定係数（Ｒ２）はいずれも０．９以上となり、非常に良好な検量線を得ることができた。 4 to 7 are calibration curves showing the relationship between the judgment value (horizontal axis) calculated by discriminants 1 to 4 and the EVOO concentration (vertical axis), respectively. The determination coefficient (R 2 ) was 0.9 or more in all cases, and a very good calibration curve could be obtained.
参考までに図４の作成に使用したデータを表１に示す。 For reference, the data used in the creation of FIG. 4 is shown in Table 1.
図４の検量線より、判別式１での判定値２００以上がＥＶＯＯ１００質量％であると判定できる。 From the calibration curve in FIG. 4, it can be determined that the determination value 200 or more in the discriminant 1 is EVOO 100 mass%.
図５の検量線より、判別式２での判定値４１以上がＥＶＯＯ１００質量％であると判定できる。 From the calibration curve in FIG. 5, it can be determined that the determination value 41 or more in the discriminant 2 is EVOO 100 mass%.
図６の検量線より、判別式３での判定値２６以上がＥＶＯＯ１００質量％であると判定できる。 From the calibration curve of FIG. 6, it can be determined that the determination value 26 or more in the discriminant 3 is EVOO 100 mass%.
図７の検量線より、判別式４での判定値１７以上がＥＶＯＯ１００質量％であると判定できる。 From the calibration curve of FIG. 7, it can be determined that the determination value 17 or more in the discriminant 4 is EVOO 100 mass%.
判定対象の油脂組成物の上記判定値を算出して上記１００質量％判定値（例えば、判別式１であれば２００以上）と比較することにより、判定対象の油脂組成物中のＥＶＯＯの含量が１００質量％であるか否かを判定できる。 By calculating the determination value of the oil / fat composition to be determined and comparing it to the 100% by mass determination value (for example, 200 or more for discriminant 1), the content of EVOO in the oil / fat composition to be determined is Whether it is 100% by mass or not can be determined.
判別式１を用い、単一食用油での判定値を算出したところ、表２に示す通りであった。 The discriminant 1 was used to calculate the judgment value for a single edible oil, which was as shown in Table 2.
ＥＶＯＯの判定値はいずれも２００以上、その他の食用油脂の判定値は２００未満であり、判別式１の有効性を確認することができた。なお、ＥＶＯＯとして販売されているにもかかわらず判定値が２００未満となる場合には、他油種がコンタミネーションしたものである可能性が高い。すなわち、判別式１はまがい物であるか否かの判定にも有効である。 The EVOO determination values were all 200 or more, and the determination values of other edible oils and fats were less than 200, and the effectiveness of discriminant 1 could be confirmed. If the judgment value is less than 200 despite being sold as EVOO, there is a high possibility that other oil types have been contaminated. That is, the discriminant 1 is also effective for determining whether or not it is a fake object.
また、海外製品における混合食用油としてクッキングオイル（ベトナム製品）について調べた結果、判定値は０．０２８であり、２００未満となり、判別式１の有効性を確認することができた。 Moreover, as a result of examining cooking oil (Vietnamese product) as a mixed edible oil in overseas products, the judgment value was 0.028, which was less than 200, and the effectiveness of discriminant 1 could be confirmed.
次に、スペイン産ＥＶＯＯに他の食用油を１質量％混合させたコンタミネーション品を作成し、判別式１にて判別できるのか調べた。結果を表３に示す。 Next, a contamination product in which 1% by mass of other edible oil was mixed with Spanish EVOO was prepared, and it was examined whether it could be discriminated by discriminant 1. The results are shown in Table 3.
表３に示した通り、いずれの検体も２００未満となり、ＥＶＯＯ１００質量％品ではないと判別することができた。本結果から、ＥＶＯＯ以外の油種が１質量％コンタミネーションしていても首尾よく判定でき、判別式１は精度の高いものと判断された。 As shown in Table 3, all specimens were less than 200, and it was possible to determine that they were not EVOO 100% by mass. From this result, even if oil types other than EVOO were contaminated by 1% by mass, it could be judged successfully, and discriminant 1 was judged to be highly accurate.
オリーブオイルの規格はＩＯＣ（国際オリーブ協会）及びＥＵ規格で定められており、紫外線吸光度K232（2.5以下）、K270（0.22以下）、ΔK（0.01以下）で特徴を決定づけている。しかし、紫外線吸光度では、以下の通りであった。
・ＥＶＯＯにマカダミアナッツオイルがコンタミネーションした場合は、見破れない。
・ＥＶＯＯにＲＯＯがコンタミネーションした場合は、ＲＯＯが５０％以上含まれていないとコンタミネーションしていることがわからない。
・ＥＶＯＯに精製ひまわり油がコンタミネーションした場合は、精製ひまわり油が５０％以上含まれていないとコンタミネーションしていることがわからない。
・ＥＶＯＯにヘーゼルナッツオイルがコンタミネーションした場合は、ヘーゼルナッツオイルが１０％以上含まれていないとコンタミネーションしていることがわからない。
・ＥＶＯＯに精製綿実油がコンタミネーションした場合は、精製綿実油５％以上含まれていないとコンタミネーションしていることがわからない。
以上より、判別式１は、同じ非破壊分析の紫外線吸光度と異なり、より良い精度で判別できるものであることがわかった。
The specifications of olive oil are determined by IOC (International Olive Association) and EU standards, and the characteristics are determined by ultraviolet absorbance K232 (2.5 or less), K270 (0.22 or less), and ΔK (0.01 or less). However, the ultraviolet absorbance was as follows.
・ If macadamia nut oil is contaminated with EVOO, it cannot be seen.
-If ROO is contaminated in EVOO, it is not known that it is contaminated unless ROO is contained in 50% or more.
・ If refined sunflower oil is contaminated in EVOO, it cannot be confirmed that the refined sunflower oil does not contain 50% or more.
・ When hazelnut oil is contaminated in EVOO, it is not known that it is contaminated unless 10% or more of hazelnut oil is contained.
・ If refined cottonseed oil is contaminated in EVOO, it cannot be known that it is contaminated unless 5% or more of refined cottonseed oil is contained.
From the above, it was found that the discriminant 1 can be discriminated with better accuracy, unlike the ultraviolet absorbance of the same nondestructive analysis.
前述の判別式２〜４についても判別式１と同様に精度の高いものと判断された。 The above discriminants 2 to 4 were determined to be highly accurate as in discriminant 1.
〔実施例２〕
（蛍光指紋の測定）
食用大豆油（精製大豆油：日清オイリオグループ株式会社製）及び／又は食用菜種油（精製キャノーラ油：日清オイリオグループ株式会社製）からなる油脂組成物の蛍光指紋を分光蛍光光度計（商品名：Ｆ−７０００、株式会社日立ハイテクサイエンス社製）により測定した。測定結果を図８に示す。
[Example 2]
(Measurement of fluorescent fingerprint)
Fluorescent fingerprint of oil composition consisting of edible soybean oil (refined soybean oil: Nisshin Oillio Group Co., Ltd.) and / or edible rapeseed oil (refined canola oil: Nisshin Oillio Group Co., Ltd.) : F-7000, manufactured by Hitachi High-Tech Science Corporation). The measurement results are shown in FIG.
図８は、種々の含量比の食用大豆油と食用菜種油とからなる油脂組成物の蛍光指紋である。各図の油脂組成物の含量比（食用大豆油：食用菜種油）は、（ａ）は０：１００、（ｂ）は１：９９、（ｃ）は２：９８、（ｄ）は１０：９０、（ｅ）は２０：８０、（ｆ）は５０：５０、（ｇ）は８０：２０、（ｈ）は９０：１０、（ｉ）は９５：５、（ｊ）は９８：２、（ｋ）は９９：１、（ｌ）は１００：０である。 FIG. 8 shows fluorescent fingerprints of an oil / fat composition comprising edible soybean oil and edible rapeseed oil in various content ratios. The content ratio (edible soybean oil: edible rapeseed oil) of the oil and fat composition in each figure is as follows: (a) 0: 100, (b) 1:99, (c) 2:98, (d) 10:90. , (E) is 20:80, (f) is 50:50, (g) is 80:20, (h) is 90:10, (i) is 95: 5, (j) is 98: 2, ( k) is 99: 1 and (l) is 100: 0.
また、各油脂組成物について２５℃における屈折率（ＲＩ）を屈折計（京都電子工業株式会社製）により測定した結果も図８に示す。 Moreover, the result of having measured the refractive index (RI) in 25 degreeC about each oil-fat composition with the refractometer (made by Kyoto Electronics Industry Co., Ltd.) is also shown in FIG.
図８から得られた情報より特徴的な蛍光強度を調査した。調査方法は、食用菜種油１００％の蛍光強度から食用大豆油１００％の蛍光強度を差し引いた結果から勘案した。その結果、食用大豆と食用菜種で異なる蛍光指紋を示している励起波長（ＥＸ）２５０〜３５０、蛍光波長（ＥＭ）２５０〜６００における範囲にて検量線を求めることとした。 The characteristic fluorescence intensity was investigated from the information obtained from FIG. The investigation method was considered from the result of subtracting the fluorescence intensity of 100% edible soybean oil from the fluorescence intensity of 100% edible rapeseed oil. As a result, the calibration curve was determined in the ranges of excitation wavelengths (EX) 250 to 350 and fluorescence wavelengths (EM) 250 to 600 showing different fluorescence fingerprints for edible soybeans and edible rapeseed.
図９は、図８（ａ）、（ｆ）、（ｌ）の蛍光指紋において、食用大豆油と食用菜種油に特徴的なピークが見られる励起波長（ＥＸ）２５０〜３５０、蛍光波長（ＥＭ）２５０〜６００の範囲（図の斜線部分）を示す図である。 FIG. 9 shows excitation wavelengths (EX) 250 to 350 and fluorescence wavelengths (EM) in which peaks characteristic to edible soybean oil and edible rapeseed oil are observed in the fluorescent fingerprints of FIGS. 8 (a), (f), and (l). It is a figure which shows the range (shaded part of a figure) of 250-600.
得られた食用菜種油１００％の蛍光強度から食用大豆油１００％の蛍光強度を引いた結果、またはその逆から求めた結果から検量線を描く。図１０に示したのは一部の結果であり、食用菜種油と食用大豆油の各配合（％）から蛍光強度をプロットして得られた検量線である。本事例を基に、他の蛍光強度にて検量線を描き、配合割合を求めることが可能である。 A calibration curve is drawn from the result obtained by subtracting the fluorescence intensity of 100% edible soybean oil from the fluorescence intensity of 100% edible rapeseed oil, or the result obtained from the opposite. FIG. 10 shows a part of the results, and is a calibration curve obtained by plotting the fluorescence intensity from each blend (%) of edible rapeseed oil and edible soybean oil. Based on this example, it is possible to draw a calibration curve at other fluorescence intensities and obtain the blending ratio.
図１０は、励起波長（ＥＸ）２８５ｎｍ、蛍光波長（ＥＭ）３３０ｎｍで測定した蛍光強度（横軸）と食用大豆油濃度（縦軸）との関係を示す検量線である。 FIG. 10 is a calibration curve showing the relationship between fluorescence intensity (horizontal axis) and edible soybean oil concentration (vertical axis) measured at an excitation wavelength (EX) of 285 nm and a fluorescence wavelength (EM) of 330 nm.
一例として挙げた図１０の検量線においては、蛍光強度＜５７．１の場合は食用大豆油１００％、蛍光強度９３．８＜の場合には食用菜種油１００％と判断することができる。 In the calibration curve of FIG. 10 given as an example, it can be determined that the edible soybean oil is 100% when the fluorescence intensity is <57.1, and the edible rapeseed oil is 100% when the fluorescence intensity is 93.8 <.
食用菜種油５検体及び食用大豆油５検体について、前述の分光蛍光光度計を用いて励起波長２８５ｎｍ、蛍光波長３３０ｎｍにて硫酸キニーネ補正をかけた蛍光強度を求めた。当該蛍光強度及び図１０の検量線からの結果を表４に示した。 For five edible rapeseed oil samples and five edible soybean oil samples, the fluorescence intensity was subjected to quinine sulfate correction at an excitation wavelength of 285 nm and a fluorescence wavelength of 330 nm using the above-described spectrofluorometer. The fluorescence intensity and the results from the calibration curve in FIG. 10 are shown in Table 4.
表４に示す結果より、図１０の検量線は概ね良好な検量線であることがわかった。なお、本結果に囚われることなく、ｎ数を増やすことでさらに良好な検量線を得ることが可能である。 From the results shown in Table 4, it was found that the calibration curve in FIG. 10 was generally a good calibration curve. It should be noted that a better calibration curve can be obtained by increasing the number of n without being bound by this result.
次に、図１０の検量線から食用調合油（食用大豆油８０％、食用菜種油２０％）について、前述の分光蛍光光度計を用いて励起波長２８５ｎｍ、蛍光波長３３０ｎｍにて硫酸キニーネ補正をかけた蛍光強度を求めた。当該蛍光強度と、図１０の検量線からの結果を表５に示した。 Next, from the calibration curve of FIG. 10, edible blended oil (edible soybean oil 80%, edible rapeseed oil 20%) was subjected to quinine sulfate correction at an excitation wavelength of 285 nm and a fluorescence wavelength of 330 nm using the aforementioned spectrofluorometer. The fluorescence intensity was determined. Table 5 shows the fluorescence intensity and the results from the calibration curve in FIG.
表５に示す結果より、図１０の検量線は概ね良好な検量線であることがわかった。 From the results shown in Table 5, it was found that the calibration curve in FIG. 10 is a generally good calibration curve.
なお、本発明は、上記実施の形態及び実施例に限定されず種々に変形実施が可能である。
In addition, this invention is not limited to the said embodiment and Example, A various deformation | transformation implementation is possible.
１：油脂Ａ、２：油脂Ｂ、３：混合油Ｃ
１０：インライン式混合装置
１１：油導入管、１１Ａ，１１Ｂ：流入口
１２：スタティックミキサー、１３：油送管、１４：分光蛍光光度計
２０：バッチ式混合装置
２１：撹拌槽、２２：攪拌機、２３：モーター
1: Oil and fat A, 2: Oil and fat B, 3: Mixed oil C
10: In-line type mixing apparatus 11: Oil introduction pipe, 11A, 11B: Inlet 12: Static mixer, 13: Oil feeding pipe, 14: Spectrofluorometer 20: Batch type mixing apparatus 21: Stirrer tank, 22: Stirrer, 23: Motor
Claims (11)
前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークの蛍光強度を測定することにより、前記油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定する判定工程と、
前記判定された含量割合が前記所望の含量割合を外れている場合に、前記混合工程において、前記所望の含量割合を下回っている方の油脂の添加量を増やす、及び／又は前記所望の含量割合を超えている方の油脂の添加量を減らす調整工程を有することを特徴とする油脂組成物の製造方法。 Oil and fat A and fat B are added so as to have a desired content ratio, mixed by a mixing device to obtain an oil and fat composition,
A determination step of determining a content ratio of the fat A and the fat B in the fat composition by measuring fluorescence intensity of one or more peaks characteristic of the fat A and / or the fat B;
In the case where the determined content ratio is out of the desired content ratio, in the mixing step, the amount of oil or fat that is less than the desired content ratio is increased, and / or the desired content ratio The manufacturing method of the oil-fat composition characterized by having the adjustment process which reduces the addition amount of the fats and oils which exceed this.
下記判定方法を用いて前記油脂組成物中の前記油脂Ａと前記油脂Ｂの含量割合を判定する判定工程と、
前記判定された含量割合が前記所望の含量割合を外れている場合に、前記混合工程において、前記所望の含量割合を下回っている方の油脂の添加量を増やす、及び／又は前記所望の含量割合を超えている方の油脂の添加量を減らす調整工程を有することを特徴とする油脂組成物の製造方法。
判定方法：油脂Ａ、油脂Ｂ、及び前記油脂Ａと前記油脂Ｂとを含む油脂組成物から選ばれる２つ以上を、分光蛍光光度計を用いて、励起波長２５０〜７００ｎｍの全部あるいは一部で励起させ、蛍光波長２５０〜８００ｎｍの全部あるいは一部を測定して得られた各蛍光指紋を比較して前記油脂Ａ及び／又は前記油脂Ｂに特徴的な１個以上のピークを選択し、分光蛍光光度計を用いて１個以上の前記ピークの波長（励起波長、蛍光波長）で判定対象の油脂組成物の蛍光強度を測定することにより、前記判定対象の油脂組成物中の前記油脂Ａ及び／又は前記油脂Ｂの含量割合を判定する。 Oil and fat A and fat B are added so as to have a desired content ratio, mixed by a mixing device to obtain an oil and fat composition,
A determination step of determining a content ratio of the fat A and the fat B in the fat composition using the following determination method;
In the case where the determined content ratio is out of the desired content ratio, in the mixing step, the amount of oil or fat that is less than the desired content ratio is increased, and / or the desired content ratio The manufacturing method of the oil-fat composition characterized by having the adjustment process which reduces the addition amount of the fats and oils which exceed this.
Judgment method: Two or more selected from fat and oil composition containing fat and oil A, fat and oil B, and the fat and oil A and the fat and oil B, using a spectrofluorimeter, all or part of the excitation wavelength of 250 to 700 nm. One or more peaks characteristic of the fats and oils A and / or the fats and oils B are selected by comparing each fluorescent fingerprint obtained by exciting and measuring all or part of the fluorescence wavelength of 250 to 800 nm, By measuring the fluorescence intensity of the oil composition to be determined at one or more wavelengths of the peak (excitation wavelength, fluorescence wavelength) using a fluorometer, the fat A and oil A in the oil composition to be determined and / Or the content ratio of the said fats and oils B is determined.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021235158A1 (en) * | 2020-05-19 | 2021-11-25 | コニカミノルタ株式会社 | Fluorescent fingerprint image acquisition device |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1038878A (en) * | 1996-07-30 | 1998-02-13 | Zenkoku Sekiyu Kyokai | Quantitative testing method of peripheral oil kind in light oil |
| JPH10128094A (en) * | 1996-10-31 | 1998-05-19 | Dainippon Screen Mfg Co Ltd | Chemical treating device for substrate |
| JP2009198124A (en) * | 2008-02-22 | 2009-09-03 | Mitsubishi Heavy Ind Ltd | Fuel monitoring device, boiler facility, and mixing ratio determining method of fuel oil |
| JP2009216525A (en) * | 2008-03-10 | 2009-09-24 | Nippon Steel Corp | Management method of factory wastewater treatment |
| JP2010185719A (en) * | 2009-02-10 | 2010-08-26 | National Agriculture & Food Research Organization | Method and apparatus for discriminating grain flour |
| WO2014181209A1 (en) * | 2013-05-06 | 2014-11-13 | Koninklijke Philips N.V. | Method and device for measuring quality and freshness of vegetable oil using fluorescence spectrophotometry |
-
2017
- 2017-02-20 JP JP2017029392A patent/JP6817844B2/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1038878A (en) * | 1996-07-30 | 1998-02-13 | Zenkoku Sekiyu Kyokai | Quantitative testing method of peripheral oil kind in light oil |
| JPH10128094A (en) * | 1996-10-31 | 1998-05-19 | Dainippon Screen Mfg Co Ltd | Chemical treating device for substrate |
| JP2009198124A (en) * | 2008-02-22 | 2009-09-03 | Mitsubishi Heavy Ind Ltd | Fuel monitoring device, boiler facility, and mixing ratio determining method of fuel oil |
| JP2009216525A (en) * | 2008-03-10 | 2009-09-24 | Nippon Steel Corp | Management method of factory wastewater treatment |
| JP2010185719A (en) * | 2009-02-10 | 2010-08-26 | National Agriculture & Food Research Organization | Method and apparatus for discriminating grain flour |
| WO2014181209A1 (en) * | 2013-05-06 | 2014-11-13 | Koninklijke Philips N.V. | Method and device for measuring quality and freshness of vegetable oil using fluorescence spectrophotometry |
Non-Patent Citations (1)
| Title |
|---|
| 堀込純: "F-7000形分光蛍光光度計を用いた蛍光指紋による食品分析技術", THE HITACHI SCIENTIFIC INSTRUMENT NEWS, vol. 58, no. 1, JPN6020015293, March 2015 (2015-03-01), pages 4982 - 4988, ISSN: 0004259166 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021235158A1 (en) * | 2020-05-19 | 2021-11-25 | コニカミノルタ株式会社 | Fluorescent fingerprint image acquisition device |
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