DESC:
FORM 2
THE PATENTS ACT 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)

1. TITLE OF THE INVENTION:
A COMPOSITION OF CALIBRATION LIQUID FOR MILK ANALYZER AND PROCESS FOR PREPARATION
2. APPLICANT:

(A) PROMPT EQUIPMENTS PVT. LTD.
(B) INDIAN
(C) 3-B, VARDAN EXCLUSIVE,
NEAR STADIUM PETROL PUMP,
NEXT TO VIMAL HOUSE
NAVRANGPURA, AHMEDABAD- 380014,
GUJARAT, INDIA

3. PREAMBLE TO THE DESCRIPTION:
PROVISIONAL
The following specification describes the invention.
þCOMPLETE
The following specification particularly describes the invention and the manner in which it is to be performed.

FIELD OF INVENTION
The present invention relates to a composition of calibration liquid for milk analyzer and process for preparation. More particularly present invention focuses on a stable calibration liquid composition and its process of preparation which mimics the properties of actual milk for estimating the milk constituents in ultrasound milk analyzer.

BACKGROUND OF INVENTION
Milk has been one of the most popular, highly nutritive and nature’s most preferred food. Milk is an important source of nutrition especially for children and infants. Milk products also form a significant part of the diet of adults around the world. It is estimatedthat at present more than 6 billion consumers use milk and milk products. As such, milk isconsidered as an important factor in improving nutrition and reducing malnutrition.The milk is composed of protein, carbohydrates, fats and trace amount of minerals and vitamins. Protein, Carbohydrates (Lactose) and mineral contents in milk are collectively known as "Solid-not-Fat" (SNF). The percentages of these contents are varying between mammals.

Conventionally, raw milk collected from dairy farms/ dairy collection center (DCS) is generally analyzed to quantify the component parts in raw milk and to assess the quality of the raw milk. The quantitative analysis of raw milk includes measurement of fat, solid not-fat (SNF), protein, minerals and water. The quantitative analysis helps in quality control and management of dairy farms. Accurate and correct measurement of milk constituents is required because:

i. The farmer / DCS receive payment on the basis of % Fat and % SNF for volume of milk poured by them.
ii. Pattern of variation in % Fat & % SNF also plays vital role in managing diet of cattle for maximum yield and predicting some diseases.

Traditional methods available for analyzing milk include chemical and infrared analysis, which are difficult to perform at a dairy farm/ Dairy collection center (DCS). Some other techniques includespectroscopic analysis of the milk in the visible wavelength range. For example, Hunter Color Method is used for quantifying amount of fat present in a milk sample. However, these techniques use expensive instruments which cannot be readily used in the dairy farms/Dairy collection center (DCS). As aresult, such instruments are confined to centralized laboratories, to which a farmer/ authorized person would periodically send milk samples for testing.

Modern techniques offer real time milk analysis using ultrasound technology. Such technology measures the velocity of the ultrasound wave passing through the sample. These Ultrasound Milk analyzers are calibrated at factory level, using primary methods. Then they are being installed at field. In the process of daily utilization of equipment there is a possibility of differing, between the results of the measuring parameters when measured by Ultrasound Milk analyzer or any other instrumental method and the corresponding primary method of analysis (Gerber for % Fat, oven dried for % SNF etc). This is a basic moment for checking the accuracy of the equipment and for making correct and precise correction and calibration. Calibration is the process by which measurement error between results of machine under test and primary method is reduced to limit of specification. When raw milk sample is being used for the calibration; it has to satisfy three basic condition:

i. Raw milk samples should cover complete range of raw milk parameters and their combinations i.e, Low Fat- Low SNF, Medium Fat- Medium SNF and High Fat-High SNF.
ii. Before using it for the calibration purpose it must be tested by defined primary methods or other equipment giving results similar to primary method. This test results are known as control value /reference value of a sample.
iii. Maintain control value of sample till calibration is completed.
In existing supply chain of raw milk, Milk analyzers are placed at various village level Dairy Collection centers (VDCS). In order to know accuracy level & need of calibration for ultrasound Milk analyzers placed at various DCS, Dairy need Calibration sample that satisfied below listed condition:
i. Sample with known values of % Fat & % SNF. These values must be decided by primary method or machine calibrated with them.
ii. Sample should not degrade or perish before the calibration process of a machine.
iii. Sample should cover compete range of % Fat and % SNF i.e. low Fat and low SNF, medium Fat and medium SNF, high Fat and high SNF required for calibration.

Accordingly, to overcome the difficulties caused by raw milk it is desperately need to invent such calibration liquid which eliminates the above mentioned drawbacks and describes a composition which depicts or mimics the properties of actual milk.

OBJECT OF INVENTION
The object of present invention is to provide a composition of calibration liquid for ultrasound milk analyzer and process for preparationfor quick and easy calibration of ultrasound milk analyzer on the fields.
Yet another object of the present invention is to provide the composition of calibration liquid for ultrasound milk analyzer and process for preparation with longer shelf life and stability.

Further object of the present invention is to provide the composition of calibration liquid for ultrasound milk analyzer and process for preparation with fat and non-fat value ranging from 2.5 to 9.7 % and 7-10 % which is similar to that of fat and non-fat content in actual milk.

Yet another object of the present invention is to provide the composition of calibration liquid for ultrasound milk analyzer and process for preparation that suits/ compatible for ultrasonic milk composition analyzer.

Another object of the present invention is to provide composition of calibration liquid for ultrasound milk analyzer and process for preparation which is preservative free and also free from stabilizing agent.

Yet another object of present invention is to provide composition of calibration liquid for ultrasound milk analyzer and process for preparation which can be kept at environment temperature during its shelf life and does not required to be heat at specific temperature in water bath before use.

SUMMARY OF INVENTTON

The present invention is directed to a composition of calibration liquid for ultrasound milk analyzer and process for preparationand which mimics the raw milk or actual milk for calibration of ultrasound milk analyzers. The present invention is directed to quick and easy calibration of the analyzer on the fields. The present invention provides composition of calibrating liquid and process of preparation for the same which is rapid, stable and easy to store as calibrating liquid. The calibration liquid is in a form of an emulsion which is preservative free, stabilizing agent free and holds a longer shelf life. The composition of calibration liquid for ultrasound milk analyzer comprises surfactant(s), distilled water, solvents, antioxidants and short/long chain fatty acids. The process for preparation of calibration liquid for ultrasound milk analyses composition comprises mixing surfactants with fatty acids and placing in water bath for few minutes. . This mixture is added in distilled water. Then it is blended with high speed blender and the liquid is homogenized to reduce the particle size and solvents are added in to the stabilized liquid as per the required value of % SNF.

DETAILED DESCRIPTION

Before explaining the present invention in detail, it is to be understood that the invention is not limited in its application to the details. The invention is capable of other embodiment and of being practiced or carried out in a variety of ways. It is to be understood that the phraseology and terminology employed herein is for the purpose of description and not of limitation.

A composition of calibration liquid for ultrasound milk analyzer and process for preparation for conducting quantitative analysis of milk components is described herein.

It is to be understood that there are four types of calibration liquid; A) buffer, B) low Fat and low SNF C) medium Fat and medium SNF D) high Fat and high SNF.
A B C D
FAT (grams) 2.5 to 3 3.5 to 4 6.5 to 7 9.2 to 9.7
SNF (grams) 7 to 7.5 8 to 8.5 9 to 9.5 9.6 to 10

The composition of calibration liquid for ultrasound milk analyzer comprises 40 gms to 100 gms of fatty acid, 4 gms to 10 gms of surfactant having HLB number in range of 4.5±0.5; surfactant having HLB number in range of 15±5 and antioxidant (33:66:1), 1200 gms to 1250 gms of distilled water and 80 gms to 110 gms of solvent.

Fatty acids are divided into four general categories: saturated, monounsaturated, polyunsaturated, and trans fats. A fatty acid is a carboxylic acid with a long aliphatic chain, which is either saturated or unsaturated. Most naturally occurring fatty acids have an unbranched chain of an even number of carbon atoms from 4 to 28. Fatty acids are usually not found in organisms but instead as three main classes of esters: triglycerides, phospholipids, and cholesteryl esters. In any of these forms, fatty acids are both important dietary sources of fuel and they are important structural components for cells.

Fatty acids are classified in various forms: by length, by saturation vs unsaturation, by even vs odd carbon content, and by linear vs branched.
1. Short-chain fatty acids (SCFA) are fatty acids with aliphatic tails of five or fewer carbons (e.g. butyric acid).
2. Medium-chain fatty acids (MCFA) are fatty acids with aliphatic tails of 6 to 12 carbons, which can form medium-chain triglycerides.
3. Long-chain fatty acids (LCFA) are fatty acids with aliphatic tails of 13 to 21 carbons.
4. Very long chain fatty acids (VLCFA) are fatty acids with aliphatic tails of 22 or more carbons.
The present applicants have found that although the use of a single long chain fatty acid has been able to provide a stable emulsion. A blend of long chain fatty acids, wherein the carbon backbone varies from C8 to C18 has been found to produce a more stable emulsion.

Surfactants are compounds that lower the surface tension (or interfacial tension) between two liquids, between a gas and a liquid, or between a liquid and a solid. Surfactants act as detergents, wetting agents, emulsifiers, foaming agents, and dispersants.

Surfactants are usually organic compounds that are amphiphilic, meaning they contain both hydrophobic groups (their tails) and hydrophilic groups (their heads). Therefore, a surfactant contains both a water-insoluble (or oil-soluble) component and a water-soluble component. Surfactants will diffuse in water and adsorb at interfaces between air and water or at the interface between oil and water, in the case where water is mixed with oil. The water-insoluble hydrophobic group extends out of the bulk water phase, into the air or into the oil phase, while the water-soluble head group remains in the water phase.

The surfactant having HLB number Hydrophilic–lipophilic balance (HLB). HLB represents the oil and water solubility of an emulsifier and is used to classify emulsifiers. The emulsifiers are also described as amphiphilic. The balance between the hydrophobic and hydrophilic properties of the molecules determines the performance of an emulsifying agent, for instance the type of emulsion formed.

The HLB number is usually on a scale of 0–20. Lower HLB values are an indication of high oil affinity. A high HLB value, on the other hand, indicates high water-solubility. As the HLB value increases, the emulsifiers become more soluble in water and their function changes from being W/O emulsifiers to being O/W emulsifiers. HLB values are useful for selecting the most appropriate type of emulsifiers for food application.

The overall purpose of antioxidants is to prevent oxidation. Synthetic antioxidants were first introduced into packaged foods. From the start, they were primarily added to edible fats and fat-containing foods for their ability to prevent food from becoming rancid and developing unpleasant odours. Synthetic antioxidants have been used in place of natural ones, mainly because they present higher stability and performance, low costs and wide availability.

Organic solvents recognized as neurotoxins include n-hexane, tetrachloroethylene, and toluene. Many classes of chemicals are used as organic solvents, including aliphatic hydrocarbons, aromatic hydrocarbons, amines, esters, ethers, ketones, and nitrated or chlorinated hydrocarbons.

Further, it is to be understood that the below procedure is for minimum batch size.

The process for preparation of calibration liquid comprises following steps:
a) Take 1200 gms to 1250 gms of distilled water and put it in the water bath till 40° C.
b) 40 gms to 100 gms of fatty acid is taken in a separate beaker.
c) Add 4 gms to 10 gms of surfactant having HLB number in range of 4.5±0.5, surfactant having HLB number in range of 15±5 and antioxidant (33:66:1) into above prepared step (b).
d) Prepared mixture of step (c) is mixed into step (b) with the help of stirrer at 40±10°C for 10±2 minutes.
e) Above prepared mixture of (d) is placed into the water bath at 40±10°C.
f) Above prepared mixture of step (e) is homogenized by high speed stirrer for 2 to 10 minutes.
g) Above homogenized mixture of step (f) into step (a) and stirred the mixture for 5 to 15 minutes.
h) Prepared mixture of step (g) is homogenized in two stage homogenizer at 160±5 bar and 45±5 bar respectively.
i) Above prepared homogenized liquid is stabilized for 1±0.5 hours at atmospheric condition;
j) Prepared stabilized liquid is mixed with 80 gms to 110 gms of solvent into above prepared stabilize liquid of step (i) as per the required value of SNF.
k) Final calibration liquid is collected.

Short chain fatty acids are selected from acetate, propionate, butyrate; saturated long-chain fatty acid includes myristic acid, palmitic acid, stearic acid, arachidic acid and cyclopropenoid.

Surfactants are selected from sorbitan laurate (Span 20), sorbitan palmitate (Span 40), sorbitan stearate (Span 60), sorbitan oleate (Span 80), polyoxyethylene sorbitan laurate (Tween 20), polyoxyethylene sorbitan palmitate (Tween 40), polyoxyethylene sorbitan stearate (Tween 60), polyoxyethylene sorbitan oleate (Tween 80), polyoxyethylene sorbitan trioleare (Tween 85), Brij 30, Brij 35, sodium oleate, potassium oleate.

Antioxidants are selected from synthetic antioxidant such as Butylated Hydroxyanisole [BHA], butylated hydroxytoluene [BHT], Propyl Gallate [PG], and Tert-Butylhydroquinone [TBHQ].

Solvents are selected from acetone, ethyl acetate, hexane, heptane, dichloromethane, methanol, ethanol, glycerol, tetrahydrofuran, acetonitrile, dimethylformamide, toluene, dimethylsulfoxide.

The prepared calibration liquid formulation composition is found to be stable and the shelf life of this prepared calibration liquid is 25±5 days.

While the present invention has been described with respect to what is presently considered to be the preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments. To the contrary, the invention is intended to cover various modifications and equivalent ranges included within the spirit and scope of those skilled in the art. It is expressly understood, however, that such modifications and range are within the spirit and scope of the present invention as set forth in the following claims.

,CLAIMS:We claim:
1. The composition of calibration liquid for ultrasound milk analyzer comprises 40 gms to 100 gms of fatty acid, 4 gms to 10 gms of surfactant having HLB number in range of 4.5±0.5; surfactant having HLB number in range of 15±5 and antioxidant (33:66:1), 1200 gms to 1250 gms of distilled water and 80 gms to 110 gms of solvent.

2. The composition of calibration liquid for ultrasound milk analyzer as claimed in claim 1, wherein fatty acids are selected from acetate, propionate, butyrate, myristic acid, palmitic acid, stearic acid, arachidic acid and cyclopropenoid.

3. The composition of calibration liquid for ultrasound milk analyzer as claimed in claim 1, wherein surfactants are selected from sorbitan laurate (Span 20), sorbitan palmitate (Span 40), sorbitan stearate (Span 60), sorbitan oleate (Span 80), polyoxyethylene sorbitan laurate (Tween 20), polyoxyethylene sorbitan palmitate (Tween 40), polyoxyethylene sorbitan stearate (Tween 60), polyoxyethylene sorbitan oleate (Tween 80), polyoxyethylene sorbitan trioleare (Tween 85), Brij 30, Brij 35, sodium oleate, potassium oleate.

4. The composition of calibration liquid for ultrasound milk analyzer as claimed in claim 1, wherein antioxidants are selected from synthetic antioxidant as Butylated Hydroxyanisole [BHA], butylated hydroxytoluene [BHT], Propyl Gallate [PG], and Tert-Butylhydroquinone [TBHQ].

5. The composition of calibration liquid for ultrasound milk analyzer as claimed in claim 1, wherein solvents are selected from acetone, ethyl acetate, hexane, heptane, dichloromethane, methanol, ethanol, glycerol, tetrahydrofuran, acetonitrile, N-N dimethylformamide, toluene, dimethylsulfoxide.

6. The composition of calibration liquid for ultrasound milk analyzer as claimed in claim 1, wherein the shelf life of calibration liquid is 25 to 30 days.

7. The process for preparation of calibration liquid comprises following steps:

a) taking 1200 gms to 1250 gms of distilled water and put it in water bath till 40 °C;
b) taking 40 gms to 100 gms of fatty acids in a separate beaker;
c) adding 4 gms to 10 gms of surfactant having HLB number 4.5±0.5; surfactant having HLB number in range of 15±5 and antioxidant (33:66:1) into above prepared step (b);
d) mixing the above prepared step (c) into step (b) with the help of stirrer at 40±10°C for 10±2 minutes.
e) placing the above prepared mixture of step (d) into water bath at 40±10 °C.
f) homogenizing the above prepared mixture of step (e) is by high speed stirrer for 2 to 10 minutes.
g) mixing the above blended mixture of step (f) into step (a) and stirring the mixture for 5 to 15 minutes;
h) homogenizing the prepared liquid of step (g) in two stage homogenizer at 160±5 bar and 45±5 bar respectively;
i) stabilizing the above prepared homogenized liquid for 1±0.5 hours at atmospheric condition;
j) adding 80 gms to 100 gms of solvent into above prepared stabilize liquid of step (i) as per the required value of SNF;
k) collecting the final calibration liquid.

Dated this on July 10, 2021