Method for measuring the binding rate between psyllium seed coat and sugar

Abstract

To observe binding with a psyllium seed coat and sugar.SOLUTION: The method for measurement includes: a first selection step of selecting an absorption band that allows a psyllium seed coat to be distinguished from other raw materials; a second selection step of selecting an absorption band that allows sugar to be distinguished from other raw materials; a first measurement step of measuring an absorption spectrum of the composition of the psyllium seed coat in a wider range of the wavenumber, the spectrum including the absorption bands selected in the first and second selection steps; a first data processing step of extracting the absorbance in the absorption bands selected in the first selection step and in the second selection step on the basis of the absorption spectrum obtained in the first measurement step; a second measurement step of determining the detection lower limit of psyllium by using the absorption band selected in the second selection step; a third measurement step of determining the detection lower limit of sugar by using the absorption band selected in the first selection step; a second data processing step of digitizing the distribution of the psyllium seed coat and the sugar by using the detection lower limits determined in the second and third measurement steps from data obtained in the first data processing step; and a calculation step of calculating the ratio of binding of the psyllium seed coat and the sugar from the distribution digitization data.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to a method for measuring the binding rate between psyllium seed coat and sugar. [Background technology]

[0002] In recent years, dietary fiber intake has decreased due to changes in eating habits. The Dietary Reference Intakes for Japanese (2020 edition) sets the target dietary fiber intake at 21g or more for men aged 18-64, 20g or more for men aged 65 and over, 18g or more for women aged 18-64, and 17g or more for women aged 65 and over. However, the 2019 National Health and Nutrition Survey reported that the daily dietary fiber intake for men in their 20s was 17.5g and 16.0g for women in their 20s, respectively, which is below the recommended intake amount.

[0003] The target intake of dietary fiber was set based on numerous reports that insufficient dietary fiber intake is associated with the onset of lifestyle-related diseases. Dietary fiber is also known to have effects such as regulating the intestines, and it is also known that there is a positive correlation between intestinal regulation and water retention. For this reason, incorporating foods enriched with dietary fiber into one's daily diet is thought to be beneficial for people who suffer from constipation or diarrhea due to poor eating habits, Westernization of eating habits, and increased stress.

[0004] Psyllium husks are one source of dietary fiber. Psyllium husks are typically dissolved in water before consumption. However, adding psyllium husks to water can easily result in clumps (lumps). Furthermore, because the surface of the clumps is hydrated and gelled, it is difficult to destroy them once they form. Therefore, a method has been adopted in which psyllium is granulated by mixing sugar or other ingredients to increase solubility (see Patent Document 1). [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Japanese Patent Application Publication No. 2017-012112 Summary of the Invention [Problem to be solved by the invention]

[0006] However, among the granulated psyllium husks, some granules are easily soluble and some are less soluble. The reason for this difference in solubility is unknown, but it is thought to be due to the binding rate of sugar attached to the psyllium. Therefore, the inventor attempted to observe the state of binding between the psyllium husks and sugars using an electron microscope. However, it is difficult to distinguish between the psyllium husks and sugars under an electron microscope, and it was virtually impossible to observe the binding between the psyllium husks and sugars. Therefore, attempts were made to distinguish between the psyllium husks and sugars using methods other than electron microscopy, but no method capable of clearly distinguishing them has been found to date. Therefore, there is currently no method for investigating the effect of the binding rate between the psyllium husks and sugars on solubility, and the above hypothesis has not yet been proven.

[0007] The present inventors have investigated methods for observing the binding between psyllium seed coats and sugars, and as a result have discovered that the use of near-infrared light makes it possible to distinguish between psyllium and sugars, which was previously impossible to distinguish between, and have thus completed the present invention. [Means for solving the problem]

[0008] To solve the above problems, the present invention provides a measurement method for measuring the binding rate of sugar to psyllium husks, comprising: a first selection step of selecting an absorption band that allows psyllium husks to be distinguished from other raw materials; a second selection step of selecting an absorption band that allows sugars to be distinguished from other raw materials; a first measurement step of measuring the absorption spectrum of the psyllium husk composition over a wider wavenumber range that includes the absorption bands selected in the first and second selection steps; a first data processing step of extracting the absorbance at the absorption bands selected in the first and second selection steps based on the absorption spectrum obtained in the first measurement step; a second measurement step of determining the lower limit of detection of psyllium husks using the absorption bands selected in the second selection step; a third measurement step of determining the lower limit of detection of sugars using the absorption bands selected in the first selection step; a second data processing step of quantifying the distribution of psyllium husks and sugars from the data obtained in the first data processing step using the lower detection limits determined in the second and third measurement steps; and a calculation step of calculating the percentage of psyllium husks bound to sugars from the quantified distribution data.

[0009] The terminology used in the claims is based on Japanese Industrial Standards (JIS) K 0212 (2016).

[0010] This configuration allows the distribution of each substance to be visualized by measuring the absorbance in the absorption bands that distinguish between psyllium husks and sugars, making it possible to distinguish between them in a way that was previously impossible with an electron microscope.

[0011] The present invention also provides a psyllium seed coat-containing composition in which, when measured using the above-mentioned measurement method, the ratio of the area occupied by psyllium seed coat to the area where psyllium seed coat is bound to sugar is 45% or more and 100% or less.

[0012] It is believed that this configuration makes it possible to obtain a composition with improved solubility in water. [Effects of the Invention]

[0013] This invention provides a method for observing the binding of sugar to psyllium seed coat without using an electron microscope. This allows the effect of the binding rate of sugar to psyllium seed coat on solubility to be investigated. Furthermore, because the rate of binding of sugar to psyllium seed coat can be measured, a consistent level of quality can be guaranteed. DETAILED DESCRIPTION OF THE INVENTION

[0014] The present invention is characterized by the use of near-infrared light absorption spectra specific to each substance to visualize and identify the distribution of a mixture of partially bound substances that cannot be identified using an electron microscope, etc. In this example, psyllium husks granulated with sugar are used as an example.

[0015] The psyllium husk used in this example is a dietary fiber material whose main component is a polysaccharide with a highly branched structure. Examples of psyllium husk used in the present invention include husks (husks) obtained from the seeds of Plantago ovata, a plant of the Plantaginaceae family, or pulverized products thereof. Examples of psyllium husks or pulverized products thereof include those commercially available as psyllium, psyllium husk, psyllium husk powder, psyllium seed gum, isagol, etc. (hereinafter referred to as "psyllium husk powder"). In the present invention, psyllium husk powder of any particle size or grade may be used, but psyllium husk powder with few impurities and high purity is preferred.

[0016] The sugars used in this example are not particularly limited, but include monosaccharides, disaccharides, and polysaccharides of trisaccharides or more. Among these, monosaccharides and disaccharides are preferred. Specific examples include glucose, fructose, sugar (sucrose), lactose, and maltose.

[0017] Psyllium husks can be granulated by conventional methods. For example, the raw material psyllium husks and sugar are weighed and thoroughly mixed. The mixed raw material powder is granulated by wet granulation. Wet granulation methods that can be used include extrusion granulation, tumbling granulation, fluidized bed granulation, and air flow granulation. Of these, it is preferable to use a fluidized bed granulation system, which can produce granules with a porous structure and high solubility.

[0018] A measurement method using near-infrared light will be described. In the present invention, measurements were carried out using a microscopic FT-IR system Spectrum400-Spotlight400 (PerkinElmer) that is capable of measurement using near-infrared light (NIR).

[0019] First, each raw material used for granulation was spread in the center of a 5 cm diameter dish to a diameter of approximately 2 cm, taking care not to overlap particles of the raw materials. Next, the NIR spectrum of each raw material used for granulation was measured using the NIR microscopy transmission method. The measurement conditions were a measurement wavenumber range of 7800 cm -1 ~4000 cm -1 , resolution 16 cm -1 The aperture size was 100 × 100 μm, the number of integrations was 16, and the background was a glass petri dish.

[0020] The NIR spectral data for each raw material was compared to identify the absorption bands that can distinguish between psyllium husk and sugar (corresponding to the "first selection step" and "second selection step" described in the claims). In this example, psyllium husk had an absorption band of 5180 cm -1 (OH stretching and OH bending bond sounds), sugars have a bond energy of 6960 cm -1 We decided to focus on the crystalline band of sucrose.

[0021] Next, the granulated material was spread over an area of ​​approximately 2 cm in diameter in the center of a 5 cm diameter dish, taking care not to overlap the particles. Next, NIR transmission imaging of the granulated material was performed using a microscopic FT-IR system Spectrum400-Spotlight400 (PerkinElmer). Measurement wavenumber range: 7200 cm-1 ~3700cm -1 , resolution 16cm -1 The measurement area was 5 mm × 5 mm, the pixel size was 25 μm, and the number of integrations was 2. Data for 40,000 pixels was obtained. Here, each pixel data had a resolution of 7,200 cm -1 ~3700cm -1 In other words, the absorption spectrum of the psyllium husk composition is measured over a wider wavenumber range, including the absorption bands selected in the first and second selection steps (this corresponds to the "first measurement step" in the claims).

[0022] Next, to quantify the absorbance peak in the absorption band selected in the first selection step, two points on either end of the peak are determined. Based on the average absorbance image, a spectrum is displayed from the average absorbance image, and the two points on either end of the absorption band of interest are selected. For psyllium husks, the -1 and 5000 cm -1 Similarly, to quantify the absorbance peak in the absorption band selected in the second selection step, two points on both ends of the peak are also determined. -1 and 6818.8 cm -1 Next, 5320.0 cm -1 ~5000cm -1 and 7076.8 cm -1 ~6818.8cm -1 This operation was performed on the absorption spectrum obtained in the first measurement step (the 40,000 pixel data previously acquired), and the absorbance data of the psyllium husks and the absorbance data of the sugars for each of the 40,000 pixels in a certain measurement area were output as two txt files (this corresponds to the "first data processing step" described in the claims).

[0023] Next, to eliminate noise during measurement, the lower limit of detection for psyllium husks and sugars was determined using the NIR transmission imaging method. The detection limit was determined using the following procedure. For psyllium husks, NIR transmission imaging was first performed on the sugars under the same conditions as when measuring the psyllium husk granules, except that the measurement area was set to 2 mm x 2 mm. From the average absorbance image of the obtained absorption spectrum, the 5320.0 cm peak, which corresponds to the absorption band of interest for psyllium husks, was determined. -1 ~5000cm -1 The area (absorbance) between the bands is extracted. From the average absorbance image obtained from the absorption band of interest in psyllium seed coat, the average value, maximum / minimum values, and standard deviation for the entire measurement area are calculated. Next, the detection limit is determined by calculating a 99% confidence interval in statistics. Here, the detection limit is calculated as 2.5 times the average value ± standard deviation. (This corresponds to the "second measurement step" described in the claims.)

[0024] Similarly, NIR transmission imaging of the psyllium husks was performed under the same conditions as when measuring the psyllium husk granules, except that the measurement area was set to 2 mm × 2 mm. The spectrum was displayed from the average absorbance image of the obtained absorption spectrum, and the 7076.8 cm band, which corresponds to the absorption band of interest for sugars, was obtained. -1 ~6818.8cm -1 The area (absorbance) between the bands is extracted. The average value, maximum / minimum values, and standard deviation of the entire measurement area are calculated from the average absorbance image obtained from the target sugar absorption band. Next, the detection limit is determined by calculating a 99% confidence interval in statistics. Here, the detection limit is calculated as 2.5 times the average value ± standard deviation (corresponding to the "third measurement step" described in the claims).

[0025] The txt file data representing the distribution of psyllium husks and sugars obtained in the first data processing step was processed using Excel using the following procedure. First, the txt data for psyllium husks and sugars were each copied to separate Excel sheets. The IF function was used to determine whether the value of each cell was greater than the lower detection limit, using the lower detection limit determined in the second measurement step for the psyllium husk data and the lower detection limit determined in the third measurement step for the sugar data (noise discrimination). The IF function was specified to return "0" if the value was below the lower detection limit, and "1" for the psyllium husk sheet and "2" for the sugar sheet if the value was greater than the lower detection limit. In other words, the determination was made using the following formulas 1 and 2 (corresponding to the "second data processing step" and "calculation step" described in the claims).

[0026] Psyllium husk data judgment = IF('Data sheet name'!Each cell>Psyllium husk detection limit, 1, 0) (Equation 1)

[0027] Sugar data judgment = IF('Data sheet name'!Each cell>Sugar detection limit, 2, 0) (Formula 2)

[0028] Next, the sum of the corresponding cells in the psyllium husk sheet and sugar sheet, which were judged to be greater than the detection limit or not, was specified to be returned to a new sheet using the following formula 3. Here, processing was performed using a commonly used method for calculating cells between multiple sheets.

[0029] = SUM('Psyllium husk determination sheet:Sugar determination sheet'!each cell) (Equation 3)

[0030] Formula 3 returns the distribution as a value: if only psyllium husks are present = 1, if only sugars are present = 2, if psyllium and sugars are present = 3, if neither psyllium nor sugars are present = 0

[0031] When psyllium and sugar are present (3), the two ingredients are defined as being in a bound mixed state, and the binding ratio of psyllium seed coat to sugar was determined using the following formula 4.

[0032] Binding rate (%) = (sugar ∧ psyllium husks) / (sugar + psyllium husks) × 100 = (number of cells containing psyllium husks and sugar) / {(number of cells containing only psyllium husks) + (number of cells containing only sugar) + (number of cells containing psyllium husks and sugar)} × 100 = (number of cells "3") / {(number of cells "1") + (number of cells "2") + (number of cells "3")} × 100 (Equation 4)

[0033] Furthermore, the "proportion of unbound psyllium seed coats," which is presumed to be the cause of the difficulty in dissolving, was calculated using the following formula 5.

[0034] Unattached psyllium husks (%) = (psyllium husks) / (sugar + psyllium husks) × 100 = (number of cells containing only psyllium husks) / {(number of cells containing only psyllium husks) + (number of cells containing only sugar) + (number of cells containing both psyllium husks and sugar)} × 100 = (number of cells "1") / {(number of cells "1") + (number of cells "2") + (number of cells "3")} × 100 (Equation 5) [Example]

[0035] Examples of the present invention will be described below, but the present invention is not limited to the following examples.

[0036] <Sample preparation> Psyllium husk powder and sucrose were mixed at the ratios shown in Table 1 to a total of 500 g. For Samples 1 to 6, after mixing, the mixture was placed in a fluidized bed granulator and granulated while spraying with water. The amount of water added was 20% of the powder weight added. After granulation, the mixture was passed through a 14-mesh Tyler sieve, and the sample was taken as the granule that passed through. Sample 1 used sucrose that did not pass through a 120-mesh Tyler sieve (sieve openings of 125 μm according to JIS standards), while Samples 2 to 6 used powdered sugar (sucrose) that passed through a 120- to 280-mesh Tyler sieve (sieve openings of 53 to 125 μm according to JIS standards). On the other hand, for sample 7, psyllium husk powder was simply mixed with powdered sugar (sucrose) that had passed through a 120-280 mesh Tyler sieve (equivalent to a sieve opening of 53-125 μm according to JIS standards), and no granulation was performed.

[0037] [Table 1]

[0038] <About binding ratio> According to the test method described above, measurements were performed on psyllium husk powder, sucrose, and each sample using a microscopic FT-IR system, Spectrum400-Spotlight400 (PerkinElmer). In this example, the lower detection limit for psyllium husk powder was 0.85 Arb, and the lower detection limit for sucrose was 0.55 Arb. Based on the obtained data, the binding ratio between psyllium husk powder and sucrose was calculated. The results are shown in Table 2. The values ​​are the average values ​​of n=4 measurement results.

[0039] <Water solubility confirmation test> The water solubility test was performed as follows. First, a 0.01 wt% concentration of Blue No. 1 dye solution was prepared. Next, 180 mL of the prepared blue dye solution and a 3 cm long stir bar were placed in a 300 mL beaker, and the beaker was then placed on a magnetic stirrer. Next, a 50 mL tube was placed in the tube using a stainless steel stand and clamp, with the opening positioned 8 cm above the water surface. Each sample was placed in the tube with the opening facing upward. Each sample weighed 6.4 g. The opening was sealed with aluminum foil, and the stir bar was rotated at 100 rpm. The tube was then rotated 180 degrees, and the aluminum cap was opened with one end still attached to the tube. Each sample was then dropped into the beaker. Immediately after dropping, the stir bar was turned off, and after waiting 30 seconds, the beaker surface was photographed in plan view. The captured image was converted to grayscale using the image analysis software ImageJ, and the area of ​​the beaker surface and the area of ​​the non-settled powder portion were determined, and the proportion of the non-settled powder portion on the beaker surface was calculated. The smaller the calculated proportion, the higher the solubility in water, i.e., the higher the affinity and ease of dissolution. The results are shown in Table 2. The values ​​are the average of n=5 measurement results.

[0040] [Table 2]

[0041] First, we investigated the effect of granulation on the binding rate between psyllium husk powder and powdered sugar (sucrose). Comparing the results for Sample 2 and Sample 7, we found that the binding rate for Sample 2, which was granulated, was 60.6%, while the binding rate for Sample 7, which was mixed only, was only 8.9%. Additionally, the rate of non-settling powder in granulated Sample 2 was 8.3%, while that for ungranulated Sample 7 was 93.4%. These results suggest that granulation increases the binding rate between psyllium husk powder and powdered sugar (sucrose), and also improves solubility.

[0042] Next, we investigated the relationship between the blending ratio and the binding ratio. As is clear from Table 2, when granulation was performed under conditions where the blending ratio of psyllium husk powder to powdered sugar (sucrose) was 1:0.37-3, the binding ratio between psyllium husk powder and sugar was 50% or more (see Samples 2-5). On the other hand, when granulation was performed under conditions where the blending ratio of sugar was greater than 3, the binding ratio between psyllium husk powder and sugar decreased (see Sample 6). Furthermore, when comparing the binding ratio between psyllium husk powder and sugar with the proportion of non-settling powder, it was found that the greater the binding ratio, the smaller the proportion of non-settling powder. In other words, the higher the binding ratio, the better the dissolution. These results suggest that a blending ratio of psyllium husk powder to powdered sugar (sucrose) of 1:0.37-3 is appropriate.

[0043] Next, we investigated the effect of sucrose particle size on the binding rate between psyllium husk powder and powdered sugar (sucrose). Comparing the results for Sample 1 and Sample 2, we found that the binding rate for Sample 1 was approximately 30%, while the binding rate for Sample 2 was 60.6%, more than double that of Sample 1. This suggests that the particle size of sucrose plays a major role in the binding rate between psyllium husk powder and sucrose.

[0044] As explained above, the present invention makes it possible to observe the binding between psyllium seed coat and sugar by visualizing and identifying psyllium seed coat and sugar, which have previously been difficult to distinguish even with an electron microscope.

Claims

1. A method for measuring the binding rate between psyllium seed coat and sugar, comprising: a first selection step of selecting an absorption band that can distinguish psyllium husks from other raw materials; a second selection step of selecting an absorption band that can distinguish sugar from other raw materials; a first measurement step of measuring the absorption spectrum of the psyllium husk composition over a wider wavenumber range that includes the absorption bands selected in the first selection step and the second selection step; a first data processing step of extracting absorbances in the absorption bands selected in the first selection step and the second selection step based on the absorption spectrum obtained in the first measurement step; a second measurement step of determining the lower limit of detection of psyllium using the absorption band selected in the first selection step; a third measurement step of determining the lower limit of detection of sugar using the absorption band selected in the second selection step; a second data processing step of quantifying the distribution of psyllium seed coats and sugars from the data obtained in the first data processing step using the detection limits determined in the second measurement step and the third measurement step; a calculation step of calculating the proportion of psyllium seed coats bound to sugar from the distribution quantification data obtained in the second data processing step; A measurement method comprising:

2. A psyllium seed coat-containing composition, in which, when measured using the measurement method described in claim 1, the ratio of the area occupied by psyllium seed coat to the area where psyllium seed coat is bound to sugar is 45% or more and 100% or less.

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