WO1992006373A1 - A method for quantitative measurement of urea in milk or a dairy product - Google Patents
A method for quantitative measurement of urea in milk or a dairy product Download PDFInfo
- Publication number
- WO1992006373A1 WO1992006373A1 PCT/FI1991/000303 FI9100303W WO9206373A1 WO 1992006373 A1 WO1992006373 A1 WO 1992006373A1 FI 9100303 W FI9100303 W FI 9100303W WO 9206373 A1 WO9206373 A1 WO 9206373A1
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- milk
- urea
- wave number
- peak
- peaks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/04—Dairy products
Definitions
- This invention relates to a method for the quantitative measurement of urea in milk or a dairy product.
- Milk is an important source of protein in the diet. Proteins are formed in the metabolism of a cow and they are secreted into the blood of the cow and also to the milk.
- the protein content of the milk in the Nordic countries is in general about 3.2-4.0% although in many other countries it is remaining smaller, often below 3%. Because of the importance of the protein it has anyhow already displaced the fat as the main basis of the price which is paid to the producers for the milk.
- the cows receive the nitrogen needed in the protein synthesis from the diet.
- the nitrogen supply is generally naturally sufficient but in the winter time when the cows are inside they are dependent on the forage which is fed to them, the nitrogen supply and with it the protein content of the milk tend to get lower.
- the cows have began in addition to milk receive urea, with the aid of which the protein content of the milk can be maintained on the level of the grazing season or even above that.
- the urea given to the cow has, anyhow, as a property that it is not totally spent in the protein synthesis but a part of it is transferred as such to the milk. Minor amounts of urea are also built up in cow's own metabolism, but the urea content depending on this is in general of magnitude at most 0.001%. In contrast to this as a consequence of the urea added to the forage the urea content of the milk can raise to 10-fold compared to the natural level or be of magnitude at most 0.01%.
- Such a high urea content is anyhow a sign of overdosing which is no more enhancing the production of protein but can instead be harmful to the health of the cow and through this to the amounts of produced milk.
- This invention has as a goal to provide a novel method for the quantitative measuring of urea in milk or a milk product wherein the above mentioned drawbacks of the prior art method have been avoided.
- the invention is characterized in that from a sample of milk or a milk product an infrared absorption spectrum is measured covering at least the peaks in the wave number area (dimension 1/cm) of about 1650-1730 and that urea is determined from the peak of it's carbon- oxygen bond peak which is at wave number of about 1651 by eliminating from this at least possible error effect of the peaks in the wave number area of carbon-oxygen bonds of aldehydes and/or ketones at about 1700-1730.
- urea determination of urea according to the invention is simple and rapid and there is no need to add any reagents to the samples to be examined.
- the results thus obtained are sufficiently accurate while the error is at most of magnitude 0.0005% and the method is well suited especially for long determination series.
- the costs of the method are essentially lower than those of the known colorimetric determination of urea.
- the usefulness of the infrared determination of urea according to the invention resides in that the milk doesn't contain such kindred materials of urea the absorption peaks of whom would be near the carbon-oxygen bound peak of urea and could hence disturb the measurement seriously. Nearest to the mentioned absorption peak of urea are situated the peaks of aldehydes and ketones present in the milk, which peaks are in the mentioned wave number area about 1700-1730. Of these substances the most abundant is acetone (absorption peak at a wave number of 1715), the concentration of which in the milk can in the case of acetonemia be over 5%.
- aldehydes and ketones present in the milk (absorption peak wave numbers in brackets), and which are formed besides as a result of an illness also as a result of the natural metabolism are e.g. benzaldehyde (1703), formaldehyde, acetaldehyde, hexyl aldehyde, nonyl aldehyde (1728), 2- butanone (1717), diacetyl, 2-pentanone (1717), 2-hexanone, 2-heptanone and 2-nonanones (1719).
- the absorption peaks of the mentioned compounds are clearly separated from the carbon-oxygen bond peak of urea, they are to some extent overlapping with the latter due to the broadening of the peaks and hence this minor error must be taken into account in the quantitative measurement numerically.
- An influence on the urea measurement have also the peak of carbon-oxygen double bond of the ester group of fats contained in the milk at a wave number of about 1748 and the peak of the peptide bond of the proteins contained in the milk at a wave number of about 1547. If the sample contains fats and/or proteins, in an accurate quantitative determination the infrared absorption spectrum has to be measured at least in the wave number area of about 1540-1760 wherein the mentioned peaks are seen and also their error effect to the urea peak at the wave number of about 1651 can be eliminated in the calculations.
- the object of the measurement of urea according to the invention can be a sample taken directly from the milked whole milk.
- In the infrared absorption spectrum are thereby visible besides of the peak of urea at a wave number of about 1651 also the nearby peaks of aldehydes, ketones, fats and proteins contained in the milk the effect of which peaks on the urea peak has to be taken into account.
- the measurement to be made is helped by homogenizing the milk prior to the measurement of the infrared spectrum so that the size of fat particles of 5-7 microns is reduced to the area between 1 and 2 microns.
- Fig. 1 is a spectrum measured from a 2% urea solution.
- Fig. 2 is a spectrum measured from whole milk containing about 3.4% fat
- Fig. 3 is a spectrum measured from fat-free (fat content 0.02-0.05%) milk.
- the absorption peak of the C 0 bond of the ester of fat at a wave number of 1748, which peak has been marked with the reference number 1
- the absorption peak of the C 0 bond of aldehydes and ketones at a wave number of about 1709, which peak has been marked with the reference number 2
- the absorption peak of the C 0 bond of urea at a wave number of about 1651, which peak has been marked with the reference number 3
- the urea can be measured quantitatively from the peak 3 of the spectrum by taking in the calculation into account the error effect of the peaks 1, 2 and 4.
- the measured wave number area 1000-2400 is as a matter of fact unnecessarily wide for the invention.
- the wave number area could in the measurement of whole milk (Fig. 2) be restricted to about 1540-1760 and in the measurement of fat- free milk (Fig. 3) possibly to a still narrower area e.g. about 1540-1730.
Abstract
The invention relates to a method for quantitative measurement of urea in milk or a milk product. The need for the measurement arises from the urea feeding of the cows the aim of which is to raise the protein content of the milk and as a consequence of which urea is also going to the milk where a large amount of it is an indication of overdosing. According to the invention an infrared absorption spectrum is measured from the sample of milk or milk product including at least the peaks in the wave number area of about 1650-1730 (1/cm), and the urea is determined from the peak of the carbon-oxygen bond at the wave number of about 1651 by eliminating from this at least the possible error effect of the peaks of the carbon-oxygen bonds of aldehydes and/or ketones in the wave number area of about 1700-1730. When the measurement is carried out in the broadened wave number area of about 1540-1760, there is also the possible peak of carbon-oxygen double bond of the ester group of fats at the wave number of about 1748 and the peak of the peptide bond of proteins at the wave number of about 1547, wherein also the possible effect of these can be taken into account.
Description
A method for quantitative measurement of urea in milk or a dairy product
This invention relates to a method for the quantitative measurement of urea in milk or a dairy product.
Milk is an important source of protein in the diet. Proteins are formed in the metabolism of a cow and they are secreted into the blood of the cow and also to the milk. The protein content of the milk in the Nordic countries is in general about 3.2-4.0% although in many other countries it is remaining smaller, often below 3%. Because of the importance of the protein it has anyhow already displaced the fat as the main basis of the price which is paid to the producers for the milk.
The cows receive the nitrogen needed in the protein synthesis from the diet. During the grazing season the nitrogen supply is generally naturally sufficient but in the winter time when the cows are inside they are dependent on the forage which is fed to them, the nitrogen supply and with it the protein content of the milk tend to get lower. In order to compensate this the cows have began in addition to milk receive urea, with the aid of which the protein content of the milk can be maintained on the level of the grazing season or even above that.
The urea given to the cow has, anyhow, as a property that it is not totally spent in the protein synthesis but a part of it is transferred as such to the milk. Minor amounts of urea are also built up in cow's own metabolism, but the urea content depending on this is in general of magnitude at most 0.001%. In contrast to this as a consequence of the urea added to the forage the urea content of the milk can raise to 10-fold compared to the natural level or be of magnitude at most 0.01%. Such a high urea content is anyhow a sign of
overdosing which is no more enhancing the production of protein but can instead be harmful to the health of the cow and through this to the amounts of produced milk.
Depending on the reasons mentioned above there has arisen a need for measuring the urea content of milk or the products produced from it. With aid of this kind of follow-up the amount of urea given to the cows can be optimized in relation to the feeding costs, the health of cows and milk production, and hence the rise of the urea content in the milk to a harmful level can be avoided.
Heretofore the quantitative measurements of urea from liquid samples have been carried out colorimetrically. This measurement is carried out by dyeing the sample with a suitable chemical and measuring the color-intensity with a colorimeter. These measurements are anyhow difficult in practice and they can't be carried out conveniently in large series. The pretreatment, the addition of reagents and the analyzing are mostly slow manual work, and the price of the reagents and labor raise the costs of the method high.
This invention has as a goal to provide a novel method for the quantitative measuring of urea in milk or a milk product wherein the above mentioned drawbacks of the prior art method have been avoided. The invention is characterized in that from a sample of milk or a milk product an infrared absorption spectrum is measured covering at least the peaks in the wave number area (dimension 1/cm) of about 1650-1730 and that urea is determined from the peak of it's carbon- oxygen bond peak which is at wave number of about 1651 by eliminating from this at least possible error effect of the peaks in the wave number area of carbon-oxygen bonds of aldehydes and/or ketones at about 1700-1730.
The determination of urea according to the invention is simple and rapid and there is no need to add any reagents to
the samples to be examined. The results thus obtained are sufficiently accurate while the error is at most of magnitude 0.0005% and the method is well suited especially for long determination series. The costs of the method are essentially lower than those of the known colorimetric determination of urea.
The usefulness of the infrared determination of urea according to the invention resides in that the milk doesn't contain such kindred materials of urea the absorption peaks of whom would be near the carbon-oxygen bound peak of urea and could hence disturb the measurement seriously. Nearest to the mentioned absorption peak of urea are situated the peaks of aldehydes and ketones present in the milk, which peaks are in the mentioned wave number area about 1700-1730. Of these substances the most abundant is acetone (absorption peak at a wave number of 1715), the concentration of which in the milk can in the case of acetonemia be over 5%. Other aldehydes and ketones present in the milk (absorption peak wave numbers in brackets), and which are formed besides as a result of an illness also as a result of the natural metabolism are e.g. benzaldehyde (1703), formaldehyde, acetaldehyde, hexyl aldehyde, nonyl aldehyde (1728), 2- butanone (1717), diacetyl, 2-pentanone (1717), 2-hexanone, 2-heptanone and 2-nonanones (1719). Although the absorption peaks of the mentioned compounds are clearly separated from the carbon-oxygen bond peak of urea, they are to some extent overlapping with the latter due to the broadening of the peaks and hence this minor error must be taken into account in the quantitative measurement numerically.
An influence on the urea measurement have also the peak of carbon-oxygen double bond of the ester group of fats contained in the milk at a wave number of about 1748 and the peak of the peptide bond of the proteins contained in the milk at a wave number of about 1547. If the sample contains fats and/or proteins, in an accurate quantitative
determination the infrared absorption spectrum has to be measured at least in the wave number area of about 1540-1760 wherein the mentioned peaks are seen and also their error effect to the urea peak at the wave number of about 1651 can be eliminated in the calculations.
There are several different methods known for measuring the fat content of milk, and one of these is the measurement of the absorption peak caused by the carbon-oxygen double bond of the ester group of fats by the infrared technique. The measuring results have been needed as the basis on which the producer is getting paid for the milk. The infrared technique hasn't, anyhow, before the present invention been used for measuring urea which is transferred to the milk directly from the feeding of the cows and the measurement of which is primarily needed for the determination of the correct feeding of the cattle.
The object of the measurement of urea according to the invention can be a sample taken directly from the milked whole milk. In the infrared absorption spectrum are thereby visible besides of the peak of urea at a wave number of about 1651 also the nearby peaks of aldehydes, ketones, fats and proteins contained in the milk the effect of which peaks on the urea peak has to be taken into account. By the whole milk the measurement to be made is helped by homogenizing the milk prior to the measurement of the infrared spectrum so that the size of fat particles of 5-7 microns is reduced to the area between 1 and 2 microns.
The quantitative measurement of urea can also be performed on fat-free milk wherein the fat peak of the spectrum has essentially disappeared. The measurement of urea according to the invention is also possible for other milk components or the products produced from the milk.
The accompanying drawings show the infrared absorption spectra measured by a MATTSSON FTIR spectrometer at a wave number area of 1000-2400, in which drawings:
Fig. 1 is a spectrum measured from a 2% urea solution.
Fig. 2 is a spectrum measured from whole milk containing about 3.4% fat, and
Fig. 3 is a spectrum measured from fat-free (fat content 0.02-0.05%) milk.
It may be mentioned that in the spectra of the figures an arrangement has been used with which the effect of the background water has been eliminated whereby the spectra are more clear-cut. This detail hasn't, anyhow, any meaning for the invention.
In the urea spectrum of Fig. 1 there is seen the absorption peak of the C=0 bond of urea at a wave number of about 1651. This peak is the basis for the measurement of urea according to the invention, though the measurement of this kind a solution containing essentially only urea is not included in the field of invention.
In the spectrum of whole milk in Fig. 2 there is seen the absorption peak of the C=0 bond of the ester of fat at a wave number of 1748, which peak has been marked with the reference number 1, the absorption peak of the C=0 bond of aldehydes and ketones at a wave number of about 1709, which peak has been marked with the reference number 2, the absorption peak of the C=0 bond of urea at a wave number of about 1651, which peak has been marked with the reference number 3, and the absorption peak of the C-N bond of proteins at a wave number of about 1547, which peak has been marked with the reference number 4. According to the invention the urea can be measured quantitatively from the
peak 3 of the spectrum by taking in the calculation into account the error effect of the peaks 1, 2 and 4.
In the spectrum of Fig. 3 of fat-free (low-fat) milk the above mentioned peaks 1, 2, 3 and 4 are, anyhow, presented so that the peak 1 caused by fat is small compared to the spectrum of Fig. 2. The measurement of urea is carried out at the urea peak 3 by taking into account the error effect arising from the other mentioned peaks 1, 2 and 4.
As can be seen from the Figures, the measured wave number area 1000-2400 is as a matter of fact unnecessarily wide for the invention. In the routine work the wave number area could in the measurement of whole milk (Fig. 2) be restricted to about 1540-1760 and in the measurement of fat- free milk (Fig. 3) possibly to a still narrower area e.g. about 1540-1730.
When a DAILAB IR-2000 spectrometer is used the amount of urea can be calculated quantitatively from the mentioned urea peak with the equation
y = 8,370x3 + 0,346x2 + 6,951x - 0,006
where y — concentration of urea and x = absorbance.
The above equation is valid as such in the case that there do not present other disturbing peaks in the neighborhood of the urea peak. While in the milk or the milk product an error which is caused by the absorption peaks 1, 2, 4 on the urea peak 3 has to been taken into account, anyhow, this is carried out with linear corrections in which the concentrations of the first mentioned peaks are multiplied by certain coefficients and reduced from the concentration value obtained from the urea peak. In the following Table the coefficients describing the effects of the mentioned substances on each other are presented.
Table
Fat Ketones + Urea Protein aldehydes
Fat 1.00 0.125 0.025
Ketones and 0.003 1.00 0.275 0.075 aldehydes
Urea 0.080 0.240 1.00 0.144
Protein 0.030 0.070 0.240 1.00
From the Table it can be seen that in the measurement of urea the correction coefficient of the fat peak is 0.125, the correction coefficient of the aldehyde and ketone peak is 0.275 and the correction coefficient of the protein peak is 0.240.
It may be mentioned, anyhow, that the invention is not restricted to the above mentioned method of calculation because there are also other methods of calculation the principles of which are familiar to one skilled in the art. Additionally it is apparent to one skilled in the art that the applications of the invention can vary within the limits which are set forth in the appended claims.
Claims
1. A method for quantitative measuring of urea in milk or a milk product, characterized in that from a sample of milk or a milk product the infrared absorption spectrum is measured including at least the peaks in the wave number area of about 1650-1730 (1/cm) and that the urea is determined from the peak of its carbon-oxygen bond at a wave number of about 1651 by eliminating from this at least the possible error effect of the peaks of carbon-oxygen bonds of aldehydes and/or ketones in the wave number area of about 1700-1730.
2. A method according to claim 1, characterized in that, the infrared absorption spectrum is measured at least in the wave number area of about 1540-1760 including besides the possible peaks of the carbon-oxygen bonds of aldehydes and ketones also the peaks of the carbon-oxygen double bond of fats optionally present in a wave number area of about 1748 and the peak of the peptide bond of proteins at a wave number of about 1547, and that the possible error effect of these peaks on the peak of the carbon-oxygen bond of urea at the wave number of about 1651 is eliminated.
3. A method according to claim 2, characterized in that urea is measured in a sample of whole milk.
4. A method according to claim 3, characterized in that urea is measured in milk which has been homogenized in order to reduce the size of the fat particles.
5. A method according to claim 1 or 2, characterized in that urea is measured in fat-free milk.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FI904880 | 1990-10-03 | ||
| FI904880A FI86480B (en) | 1990-10-03 | 1990-10-03 | FOERFARANDE FOER KVANTITATIV BESTAEMNING AV UREA FRAON MJOELK ELLER EN MJOELKPRODUKT. |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1992006373A1 true WO1992006373A1 (en) | 1992-04-16 |
Family
ID=8531166
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/FI1991/000303 WO1992006373A1 (en) | 1990-10-03 | 1991-10-02 | A method for quantitative measurement of urea in milk or a dairy product |
Country Status (2)
| Country | Link |
|---|---|
| FI (1) | FI86480B (en) |
| WO (1) | WO1992006373A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993019364A1 (en) * | 1992-03-25 | 1993-09-30 | A/S Foss Electric | A method for determining urea in milk |
| AU654933B3 (en) * | 1992-03-25 | 1994-11-24 | Foss Electric A/S | A method for determining urea in milk |
| CN102539421A (en) * | 2010-12-21 | 2012-07-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for qualitatively detecting urea in milk |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4447725A (en) * | 1981-06-15 | 1984-05-08 | Biggs Delmar A | Quantitative measurement of fat, protein and lactose in dairy products |
| DE3420987A1 (en) * | 1984-06-06 | 1985-12-19 | Klaus-Ingo Dr. 7944 Herbertingen Arnstadt | DETERMINATION OF MILK'S UREA CONTENT |
| EP0382908A2 (en) * | 1989-02-16 | 1990-08-22 | Anadis Instruments S.A. | Ir-spectrometric analysing procedure and means |
-
1990
- 1990-10-03 FI FI904880A patent/FI86480B/en not_active Application Discontinuation
-
1991
- 1991-10-02 WO PCT/FI1991/000303 patent/WO1992006373A1/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4447725A (en) * | 1981-06-15 | 1984-05-08 | Biggs Delmar A | Quantitative measurement of fat, protein and lactose in dairy products |
| DE3420987A1 (en) * | 1984-06-06 | 1985-12-19 | Klaus-Ingo Dr. 7944 Herbertingen Arnstadt | DETERMINATION OF MILK'S UREA CONTENT |
| EP0382908A2 (en) * | 1989-02-16 | 1990-08-22 | Anadis Instruments S.A. | Ir-spectrometric analysing procedure and means |
Non-Patent Citations (1)
| Title |
|---|
| CHEMICAL ABSTRACTS, Volume 100, No. 21, 21 May 1984, (Columbus, Ohio, US), KYLA-SIUROLA, A.L. et al., "The composition of milk: the determination of protein by the infrared method", see page 513, abstract 173348f; & MEIJERITIET. AIKAK. 1983, 41(2), 40-55. * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993019364A1 (en) * | 1992-03-25 | 1993-09-30 | A/S Foss Electric | A method for determining urea in milk |
| US5252829A (en) * | 1992-03-25 | 1993-10-12 | A/S Foss Electric | Method of determining urea in milk |
| AU654933B3 (en) * | 1992-03-25 | 1994-11-24 | Foss Electric A/S | A method for determining urea in milk |
| AU655110B2 (en) * | 1992-03-25 | 1994-12-01 | Foss Electric A/S | A method for determining urea in milk |
| CN102539421A (en) * | 2010-12-21 | 2012-07-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for qualitatively detecting urea in milk |
Also Published As
| Publication number | Publication date |
|---|---|
| FI904880A (en) | 1992-04-04 |
| FI86480B (en) | 1992-05-15 |
| FI904880A0 (en) | 1990-10-03 |
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