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					CERTIFICATE OF ANALYSIS
PRODUCT BATCH NO. PRODUCTION DATE EXPIRY DATE STANDARD : : : : : CHOLINE CHLORIDE 60% CORN COB HC60Y0701028 OCT, 2007 OCT, 2009 HG2941-1999

------------------------------------------------------------------------------------------------------------------------------WE HAVE INSPECTED THE QUALITY OF THE ABOVE MENTIONED GOODS AND FOUND THE RESULT OF INSPECTION AS FOLLOWS :

ITEMS CONTENT % CARRIER LOSS ON DRYING % PARTICLE SIZE %(THROUGH 20 MESH SIEVE) TMA PPM

SPECIFICATIONS 60.04 CORN COB 1.5 95.01 197

RESULTS ≥60% CORN COB ≤2% ≥95% ≤300

CONCLUSION: ALL OF THE ITEMS COMPLY WITH THE REQUIREMENT OF HG2941-1999

NOTE: ANALYSIS METHOD OF CHOLINE CHLORIDE (Ⅰ) REINECKE SALT GRAVIMETRIC METHOD
The Principle of the Reinecke Salt Gravimetric Method is hot water extraction of choline chloride from the sample. Dilute and boil with NaOH to remove possible primary, secondary and tertiary amines. Adjust pH to 4-6. React with Reineckle salt solution to form precipitate and compute the choline chloride content. The reagents needed are : • • • • 40 % of Sodium hydroxide solution Hydrochloric acid concentrate 3 mol/L of Hydrochloric acid solution 2 % of Reinecke salt/Methanol solution.

•

Methyl Red indicator.

The Apparatus needed are : 1) Analytical balance 2) Water bath 3) Electrical shaker 4) Filtering flask with 30mL crucible filter G4, which is equivalent to international standard P7 model 5) Drying oven Analytical procedures First, let us look at the powder sample Take 5 - 10 g of sample. Put them into a small beaker. Dry up in oven at 105 º C till constant weight. This will normally take about 2 – 3 hours. Take about 1 g of the dried sample. Precision to a level of ± 0.2 mg. Put it in a 100ml flask and add 70 ml of water. Stir and heat it up in water with a temperature of 70 ± 3 º C for about 15 minutes. Shake using an electric shaker for about 10 minutes. Cool down to room temperature and add water to make up to 100ml and filter. Precisely put 10ml of the filtered solution in a 100ml beaker. Add in 3ml of sodium hydroxide solution and stir. Place a funnel on the beaker and boil for 5 minutes on an electric stove. Remove and rinse the beaker and funnel with water. Add in 2 drops of Methyl Red indicator and using Hydrochloric acid concentrate and Hydrochloric acid solution to adjust pH of the solution to 4 – 6, indicated by the change of the solution color from yellow to red. Filter quantitatively if necessary. Cool the solution in ice- water for 5 minutes. While stirring, add in slowly15ml of Reinecke salt/Methanol solution. Stir for 30 minutes and let it precipitate and settle for another 30 minutes in a refrigerator. Filter the solution quantitatively by suction through a filter crucible that was earlier on, oven dried at 105 º C to constant weight. The filtered solution should be cleared. Wash the filtrate 3 – 4 times with water and oven dried together with the crucible filter at 105 º C for about 2 hours. Measure the weight.

And For the Liquid samples Take about 0.7g of sample (precision to ± 0.2mg). Put them in a 100ml flask and make up with water to 100ml. Stir well. Precisely take 10ml of the

solution and place them in a 100ml beaker. The subsequent procedures are similar to the powder sample.

The Calculation Formula The formula to compute the content of choline chloride in the sample is : 0.33045x10x ( m2-m1) X(%)= m Where : X = The percentage of Choline chloride in the sample m = The weight of the sample (g) m1 = the weight of the oven dried crucible filter m2 = the weight of the oven fried crucible filter with precipitate 0.33045: conversion rate

(Ⅱ) AgNo3 titration method
ACTIVE INGREDIENT 1.1 ACTIVE INGREDIENT DESCRIBED BY A PHARMACOPOEIA CHOLINE CHLORIDE 1.2 SCIENTIFIC DATA ITEM TARGET Aqueous solution 70% CHOLINE CHLORIDE CONTENT≥ PH GLYCOL CONTENT≤ TRIMETHYLAMINE≤ ASH≤ HEVEY METAL(Pb) CONTENT≤ 1.2.1 NOMENCLATURE CHOLINE CHLORIDE 1.2.2 DESCRIPTION 1.2.2.1 Choline chloride aqueous solution is transparent dauby solution without color. It has a little special stink. It can be mixed with water, carbinol, ethanol at discretion, but it can hardly be mixed with aether, benzene. It has the character of moisture absorption and it will release amic, when it absorbs carbon dioxide. 1.2.2.2Choline chloride powder is white or filemit dry floating powder or grain.(The colour is changed by the carrier).It has the character of moisture absorption and has special stink. 70.0 6.0~8.0 0.50 0.10 0.20 0.002 75% 75.0 6.0~8.0 0.50 0.10 0.20 0.002 Powder 50% 50.0 — — 0.10 — — 60% 60.0 — — 0.10 — —

1.2.3 PRODUCTION 1.2.3.1Choline chloride aqueous solution is produced by the reaction of trimethylamine muriatic acid aqueous solution and epoxy ethane. 1.2.3.2Choline chloride powder : The choline chloride aqueous solution is added with carrier(such as corncob, brain, ect.)and it was dried. So the choline chloride powder comes into being. 1.2.4 Quality Control During Manufacture We control the quality according to the requirement of ISO9001:2000 stictly during manufacture. 1.2.5 Development Chemistry CH3 CH3

CH3

N

CH3 + HCL ≤600C,PH 6~7

[H

N+ CH3

CH3 ]CL¯

CH3

CH3

[H

N+ CH3

CH3 ]CL¯

+

CH2 O

CH2

≤450C PH10~11

[H

N+ CH2 CH2 CH2

CH3 ]CL¯

1.2.6Impurities Glycol Trimethylamine Heavy Metal 1.2.7. Batch Analysis There will be a batch analysis report for every batch. 2.STABILITY TESTS ON THE ACTIVE INGREDIENT We carry out the tests on the active ingredient according to the requirement of HG2941-1999. 3.TEST METHOD----AgNo3 titration method. 3.1.1 principium It tests choline chloride by testing the content of Cl-. Chromium acid potassium is taken as the indicator ,The solubility of Agcl is weaker than the solubility of chromium acid silver. Using AgNo3 to titrate chloride hydronium, it is the end, when brick red chromium acid silver appears. 3.1.2 reagent and material AgNo3 solution:0.1mol/L , chromium acid potassium indicator100g/L

3.1.3 Test step for 75% choline chloride Weigh 0.5g(precision:0.0002g) test sample, put it into 250mL iodine measuring flask, add 50mL water and shake it symmetrically. Add 0.5mL Chromium acid potassium,. It is the end, when brick red chromium acid silver appears. 3.1.4 Calculation C2(v4-v3)x0.139 6 X7= ×100 ……………………………………………………………………(A1) M11 MARKS: X7 is the content of choline chloride C2-----The real concentration of AgNo3 standard indicator solution. Mol/L. v4…….The cubage of the depleted AgNo3 standard indicator solution by the test sample.. v3………. The cubage of the depleted AgNo3 standard indicator solution by the blank test. M11…….the mass of test sample, g. 0.139 6……The mass of choline chloride by g ,which is equal to 1.00mL AgNo3 titration solution[c(AgNo3)=1.000mol/L] 3.1.2 Test step for CHOLINE CHLORIDE 60% Weigh 1.2g(precision:0.0002g) test sample, which is dried under 1050C. Put it into 100mL capacity bottle., add water to dilute it to 100mL. Shake it symmetrically. Lay it for 20minutes. Filtrate the solution. Give up the primary filtrating solution. Put 50.0mL test sample solution into subulate bottle . Add 0.5mL Chromium acid potassium, Then operate same as 3.1.3 3.1.3Error allowed: 1% more or less is allowed


				
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