Wheat Gluten. Wheat Protein Isolate

Transcription

1 500 / Wheat Gluten / Monographs FCC V Preparation, and R U and R S are the relative peak response ratios for the Assay Preparation and the Standard Preparation, respectively. Calculate R U and R S by the formula (r Z + r E )/r I, in which r Z is the response for the (Z)-phytonadione peak, r E is the response for the (E)-phytonadione peak, and r I is the response for cholesteryl benzoate in the Internal Standard peak. Lead Determine as directed in the Flame Atomic Absorption Spectrophotometric Method under Lead Limit Test, Appendix IIIB, using a 10-g sample. Menadione Mix about 20 mg of sample with 0.5 ml of a 1:1 (v/v) mixture of 6 N ammonium hydroxide:alcohol, add 1 drop of ethyl cyanoacetate, and shake gently. No purple or blue color appears. Refractive Index Determine as directed under Refractive Index, Appendix IIB, using an Abbé or other refractometer of equal or greater accuracy. (Z) Isomer Content (Note: Protect solutions containing Vitamin K from exposure to light.) Mobile Phase, Internal Standard, Assay Preparation, Chromatographic System, and Procedure Determine as directed in the Assay, except calculate the percentage of (Z) isomer taken by the formula 100r Z /(r Z + r E ), in which r Z is the peak area of the (Z)-phytonadione isomer peak and r E is the peak area of the (E)-phytonadione isomer peak obtained from the Assay Preparation. Store in tight, light-resistant con- tainers. viscoelastic mass, which can be lifted with the stirring rod without breaking apart. Devitalized Wheat Gluten will not form such a mass. Assay Not less than 71.0% protein, calculated on the dried basis. Ash (Total) Not more than 2.0%, calculated on the dried basis. Crude Fat Not more than 2.0%. Lead Not more than 1 mg/kg. Loss on Drying Not more than 10.0%. Starch Not more than 21.0%. Assay Determine as directed under Nitrogen Determination, Appendix IIIC. Calculate the percent protein by the formula 5.7 N, in which N is the percent of nitrogen. Ash (Total) Determine as directed under Ash (Total), Appendix IIC. Crude Fat Determine as directed under Crude Fat, Appendix X. Lead Determine as directed for Method I in the Atomic Lead Limit Test, Appendix IIIB, using a 1-g sample. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying a 2-g sample at 105 for 2 h. Starch The remainder, after subtracting from 100.0% the sum of the percents of Ash (Total), Loss on Drying, and Protein (see Assay, above), represents the percent of starch in the sample. Store in well-closed containers. Wheat Gluten Vital Wheat Gluten; Devitalized Wheat Gluten CAS: [ ] Wheat Gluten occurs as a cream to light tan, free-flowing powder. It is the water-insoluble complex protein obtained by water extraction of wheat or wheat flour. It is soluble in alkalies, and partly soluble in alcohol and dilute acids. Vital Wheat Gluten is characterized by high viscoelasticity when hydrated, while Devitalized Wheat Gluten has lost this character because of denaturation by heat. Dough strengthener; nutrient; stabilizer and thickener; surface-finishing agent; and texturizing agent. Identification Add 40 ml of room-temperature water to 20 g of sample, and stir. Vital Wheat Gluten will form a cohesive, Wheat Protein Isolate Wheat Protein Isolate occurs as a powder. It is produced by acidic deamidation of gluten that converts glutamine and asparagine to their nonamidated derivatives, glutamic acid and aspartic acid, followed by several purification measures. Alternatively, gluten can be solubilized in an acidic or alkaline medium, and the dissolved protein is then separated and purified by filtration or centrifugation. Texturizer; nutrient; emulsifier; water-binding aid; gelling agent; foaming agent. Note: Calculate all analyses, except those for Loss on Drying, on the dried basis, drying to constant weight at 130.

2 FCC V Monographs / Whey / 501 Labeling Indicate the protein content. Identification Wheat Protein Isolate exhibits the compositional profile specified below with respect to Ash, Fat, Loss on Drying, and Protein. Assay (as Protein) Not less than 75% protein. Ash (Total) Not more than 8%. Fat Not more than 6%. Loss on Drying Not more than 10%. ph of a 10% Solution Between 4.3 and 7.5. Assay (as Protein) Determine the percent nitrogen as directed under Nitrogen Determination, Appendix IIIC, or by the Protein Nitrogen Combustion Method, AOAC or AOCS Ba 4e-93. The percent protein equals percent N 5.7 and is calculated to exclude added vitamins, minerals, amino acids, and food additives. Ash (Total) Determine as directed under Ash (Total), Appendix IIC, to a final gray to white residue. Fat Determine as directed under Crude Fat, Appendix X. Lead Determine as directed for Method I in the Atomic Lead Limit Test, Appendix IIIB. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying a 2-g sample at 65 at a pressure of less than 100 mm Hg for 16 h. ph of a 10% Solution Determine as directed under ph Determination, Appendix IIB, using a 10% aqueous solution. Whey Whey is the liquid obtained by separating the coagulum from milk, cream, and/or skim milk in cheese making. Whey obtained from the process in which a significant amount of lactose is converted to lactic acid or obtained from the curd formed by direct acidification of milk is known as acid-type Whey. Whey obtained from the process in which there is insignificant conversion of lactose to lactic acid is known as sweet-type Whey. The acidity of Whey may be adjusted by the addition of safe and suitable ph-adjusting ingredients. The final product is pasteurized and is available as a liquid or dry product. Texturizer; nutrient. Note: Calculate all analyses, except those for Loss on Drying, on the dry basis. Labeling State whether the product is sweet or acid, if the product is liquid, and the concentration, as total solids based on the value obtained under Loss on Drying (below). Identification Whey exhibits the compositional profile specified below with respect to Ash, Fat, Lactose, Loss on Drying, and Protein. Ash (Total) Between 7.0% and 14.0%. Fat Between 0.2% and 2.0%. Lactose Between 61.0% and 75.0%. Loss on Drying Dry Product: Not more than 5.0%; Liquid Product: Not more than 95.0%. Protein Between 10.0% and 15.0%. Titratable Acidity (as Lactic Acid) Sweet-Type Whey: Not more than 0.16%; Acid-Type Whey: Not less than 0.35%. Ash (Total) Proceed as directed under Ash (Total), Appendix IIC, to a final gray to white residue. Fat Transfer 1gofsample, accurately weighed, into a fatextraction flask, add 10 ml of water, and shake until homogeneous (warm if necessary). Add approximately 1 ml of ammonium hydroxide, and heat in a water bath for 15 min at 60 to 70, shaking occasionally. Add 10 ml of alcohol, and mix well. Add 25 ml of peroxide-free ether, stopper, and shake vigorously for 1 min; allow to cool if necessary; add 25 ml of petroleum ether; and shake vigorously. Allow the layers to separate and clarify, or centrifuge at 600 rpm to expedite the process. Decant the organic layer into a suitable flask or dish, and repeat the extraction twice with 15 ml each of ether and petroleum ether for each extraction. Evaporate the combined ether extractions on a steam bath, and dry the residue to a constant weight at 102, or 70 to 75 at less than 50 mm Hg. Calculate the percent of fat in the sample taken by the formula (R 100)/S, in which R is the weight, in milligrams, of the residue; and S is the weight, in milligrams, of the sample taken. Lactose Mobile Phase Use a filtered and degassed 80:20 acetonitrile:water mixture at a flow rate of 2 ml/min. Internal Standard Solution Prepare an aqueous solution of USP Fructose Reference Standard having a concentration of 100 mg/ml. Standard Solution Using an accurately weighed quantity of USP Lactose Reference Standard, prepare a solution in water having a concentration of 20 mg/ml. Dilute 9 volumes of this solution with 1 volume of the Internal Standard Solution to obtain a Standard Solution having a known concentration of 18 mg of USP Lactose Reference Standard per milliliter. Prepare fresh daily. Assay Preparation Transfer an accurately weighed quantity of sample containing about 180 mg of lactose into a 10- ml volumetric flask, add 1 ml of the Internal Standard Solution, dilute with water to volume, and mix. Chromatographic System (See Chromatography, Appendix IIA.) Use a suitable high-performance liquid chromato-

3 502 / Whey Protein Concentrate / Monographs FCC V graphic system operated at room temperature and equipped with a differential refractometer detector and a 250-mm 4.6-mm (id) microparticle silica gel with siloxane bonded cyano-amino moieties (Whatman P-10 carbohydrate, or equivalent) column. Inject a 25- L portion of the Standard Solution and record the peak responses. Replicate injections show a relative standard deviation of not more than 2.0% for the ratio of the response of lactose to that of the internal standard. Procedure Separately inject 25- L portions of the Assay Preparation and the Standard Preparation into the chromatograph and record the responses. Calculate the percent lactose in the sample taken by the formula (10C S /W)(R U /R S ), in which C S is the concentration, in milligrams per milliliter, of USP Lactose Reference Standard in the Standard Solution; W is the weight, in milligrams, of sample taken; and R U and R S are the response ratios of lactose to the Internal Standard Solution obtained with the Assay Preparation and the Standard Solution, respectively. Correct to the dried basis using the value obtained under Loss on Drying (below). Lead Determine as directed for Method II in the Atomic Lead Limit Test, Appendix IIIB. Loss on Drying Dry Product: Dry a 2-g sample at 65 at a pressure of less than 100 mm Hg for 16 h. Liquid Product: Evaporate to dryness on a steam bath, and continue as directed for the dry product. Protein Determine the percent of nitrogen as directed under Nitrogen Determination, Appendix IIIC. Calculate the percent protein by the formula N 6.38, in which N is the percent nitrogen. Titratable Acidity (as Lactic Acid) Accurately weigh a portion of the finely ground dry sample or liquid equivalent to 10.0 g of total solids based on the value obtained under Loss on Drying (above), and transfer into a 500-mL conical flask. Add 100 ml of carbon dioxide-free water, and stir for 1 min. Allow to stand for 1hatroom temperature. Add 0.5 ml of phenolphthalein TS, and titrate with 0.1 N sodium hydroxide to a pink endpoint that persists for 30 s. Each milliliter of 0.1 N sodium hydroxide is equivalent to mg of lactic acid. Whey Protein Concentrate occurs as either a liquid or a dry product. It is the substance obtained by the removal of sufficient nonprotein constituents from whey so that the finished dry product contains not less than 25.0% protein. Whey Protein Concentrate is produced by physical separation techniques such as precipitation, filtration, or dialysis. The acidity of the Whey Protein Concentrate may be adjusted by the addition of safe and suitable ph-adjusting ingredients. The final product is pasteurized. Texturizer; nutrient; emulsifier; water-binding aid; gelling agent. Note: Calculate all analyses on a dry basis. Evaporate Labeling Indicate the concentration of protein and, if the product is liquid, the concentration, as total solids, based on the value obtained under Loss on Drying (below). Identification Whey Protein Concentrate exhibits the compositional Ash (Total) Between 2.0% and 15.0%. Fat Between 0.2% and 10.0%. Lactose Not more than 60.0%. Loss on Drying Dry Product: Not more than 6.0%. ph Between 6.0 and 7.2. Protein Not less than 25.0% and not more than 89.9%. Proceed as directed in the monograph for Whey. Whey Protein Isolate Whey Protein Concentrate Whey Protein Isolate occurs either as a liquid or as a dry product. It is the substance obtained by the removal of sufficient nonprotein constituents from whey so that the finished dry product contains not less than 90% protein. Removal of nonprotein constituents is accomplished by separation techniques such as precipitation, membrane filtration, and/or ion exchange. The acidity of Whey Protein Isolate may be adjusted by the addition of safe and suitable ph-adjusting ingredients. The final product is pasteurized.

4 FCC V Monographs / Whey, Reduced Minerals / 503 Source of high-quality protein; gelling agent; water-binding aid; foaming or whipping aid; emulsifier; edible coating used as a moisture barrier. Note: Perform all analyses, except that for Loss on Drying, on the dry basis. Evaporate liquid samples to dryness on a steam bath; then as for dry samples, dry to constant weight at 65 under Labeling Indicate the concentration of protein and, if the product is liquid, state the concentration, as total solids, based on the value obtained under Loss on Drying (below). Identification Whey Protein Isolate exhibits the compositional Fat, Lactose, Loss on Drying, and Protein. Ash Less than 6.0%. Fat Less than 6.0%. Lactose Not more than 6.0%. Loss on Drying Dry Product: Not more than 6.0%. ph Between 6.0 and 7.2. Protein Not less than 90.0%. IIB, using a 10% aqueous solution if the sample is in the Whey, Reduced Lactose Whey, Reduced Lactose, occurs as either a liquid or a dry product. It is the substance obtained by the selective removal of lactose from whey. Removal of lactose is accomplished by physical separation techniques such as precipitation, filtration, or dialysis. The acidity of Reduced Lactose Whey may be adjusted by the addition of safe and suitable ph-adjusting ingredients. The final product is pasteurized. Texturizer; nutrient; emulsifier. Note: Perform all analyses on a dry basis. Evaporate Labeling If the product is liquid, indicate the concentration, as total solids, based on the value obtained under Loss on Drying. Identification Reduced Lactose Whey exhibits the compositional Ash (Total) Between 11.0% and 27.0%. Fat Between 0.2% and 4.0%. Lactose Not more than 60.0%. Loss on Drying Dry Product: Not more than 4.0%. ph Between 5.5 and 7.2. Protein Between 16.0% and 24.0%. Whey, Reduced Minerals Whey, Reduced Minerals, occurs as either a liquid or a dry product. It is the substance obtained by the removal of a portion of the minerals from whey. Reduced Minerals Whey is produced by physical separation techniques such as precipitation, filtration, ion exchange, or dialysis. The acidity of the Reduced Minerals Whey may be adjusted by the addition of safe and suitable ph-adjusting ingredients. The final product is pasteurized. Texturizer; nutrient. Note: Perform all analyses on a dry basis. Evaporate Labeling If the product is liquid, indicate the concentration as total solids based on the value obtained under Loss on Drying. Identification Whey, Reduced Minerals, exhibits the compositional Ash (Total) Not more than 7.0%. Fat Between 0.2% and 4.0%.

5 504 / Wintergreen Oil / Monographs FCC V Lactose Not more than 85.0%. Loss on Drying Dry product: Not more than 4.0%. ph Between 6.2 and 7.2. Protein Between 10.0% and 24.0%. Wintergreen Oil Assay Determine as directed in Ester Determination under Esters, Appendix VI, using about 2gofsample, accurately weighed, and as the equivalence factor (e) in the calculation. Modify the procedure by using 50.0 ml of 0.5 N alcoholic potassium hydroxide and by refluxing on the steam bath for 2h. Acid Value Determine as directed under Acid Value, Appendix VI, using bromocresol purple TS as the indicator instead of phenolphthalein TS. Angular Rotation Determine as directed under Optical (Specific) Rotation, Appendix IIB, using a 100-mm tube. Refractive Index Determine as directed under Refractive Index, Appendix IIB, using an Abbé or other refractometer of equal or greater accuracy. Solubility in Alcohol Determine as directed under Solubility in Alcohol, Appendix VI. One milliliter of sample dissolves in 7 ml of 70% alcohol. The solution may have not more than a slight cloudiness. Specific Gravity Determine by any reliable method (see General Provisions). Gaultheria Oil CAS: [ ] Store in a cool place protected from light in full, tight containers. Wintergreen Oil occurs as a colorless to yellow liquid with the characteristic odor and taste of wintergreen. It is obtained by maceration and subsequent distillation with steam from the leaves of Gualtheria procumbens L. (Fam. Ericaceae) or from the bark of Betula lenta L. (Fam. Betulaceae). It boils, with decomposition, between 219 and 224. It is soluble in alcohol and in glacial acetic acid, and it is very slightly soluble in water. Flavoring agent. View IR Identification A. Shake 1 drop of sample with about 5 ml of water, and add 1 drop of ferric chloride TS. A deep violet color appears. B. The infrared absorption spectrum of the sample exhibits relative maxima at the same wavelengths as those of a typical spectrum as shown in the section on Infrared Spectra, using the same test conditions as specified therein. Assay Not less than 98.0% and not more than 100.5% of methyl salicylate (C 8 H 8 O 3 ). Acid Value Not more than 1.0. Angular Rotation Slightly levorotatory, exhibiting a rotation of not more than 1.5. Refractive Index Between and at 20. Solubility in Alcohol Passes test. Specific Gravity Between and Xanthan Gum INS: 415 CAS: [ ] Xanthan Gum occurs as a cream colored powder. It is a highmolecular-weight polysaccharide gum produced by a pureculture fermentation of a carbohydrate with Xanthomonas campestris, purified by recovery with isopropyl alcohol, dried, and milled. It contains D-glucose and D-mannose as the dominant hexose units, along with D-glucuronic acid and pyruvic acid, and it is prepared as the sodium, potassium, or calcium salt. It is readily soluble in hot or cold water, but it is insoluble in alcohol. Its solutions are neutral. Stabilizer; thickener; emulsifier; suspending agent; bodying agent; foam enhancer. Identification Transfer 300 ml of water, previously heated to 80, into a 400-mL beaker and stir rapidly with a mechanical stirrer. At the point of maximum agitation, add a dry blend of 1.5 g of sample and 1.5 g of locust bean gum. Stir until the mixture goes into solution, and then continue stirring for 30 min longer. Do not allow the water temperature to drop below 60. Discontinue stirring, and allow the mixture to cool