Mannitol Inspection Operating Procedures
No. STP–JY––004–01 Title Mannitol Inspection Operating Procedures Page Number*** 4 pages
Reviewed by the drafter Person Approval Person Execution Date
Date Date Date Revision Date
Drafting Department
Distribution Department
Purpose: To check the quality of mannitol raw materials Whether the quality complies with the provisions of Part II of the 2000 edition of the Chinese Pharmacopoeia, this procedure is compiled.
Scope: Testing of mannitol.
Responsible persons: Director and laboratory technician of the central laboratory.
Procedures:
4.1. Inspection product name: Mannitol
Molecular formula: C6H14O6
Molecular weight: 182.17
4.2. Compilation basis: Chinese Pharmacopoeia 2000 Edition, Part 2
4.3. Sampling method: Sampling according to material sampling procedures.
4.4. Inspection items: properties, identification, inspection, and content determination.
4.4.1. Inspection instruments:
4.4.1.1. Equipment: automatic electric thermostat, muffle furnace.
4.4.1.2. Instruments: melting point tester, infrared spectrometer, rack balance, analytical balance.
4.4.1.3. Reagents and reagents: acetyl chloride, pyridine, ether, ferric chloride, sodium hydroxide, phenolphthalein, sodium chloride, potassium sulfate, concentrated ammonia, calcium chloride, sodium oxalate , sulfuric acid, potassium bromide bromine test solution, sodium periodate, starch, sodium sulfate sulfate, potassium iodide.
4.4.2. Properties
This product is a white crystalline powder, odorless, sweet, easily soluble in water, and almost insoluble in ethanol or ether.
4.4.2.1. Melting point: The melting point of this product is 166~170℃. Check according to the melting point inspection procedures.
4.4.2.2. Identification: Take about 0.5g of this product, place it in a test tube, add 3ml of acetyl chloride, slowly add 0.5ml of pyridine dropwise, and shake with the drops. Once the reaction is completed, pay attention to Move the solution to another test tube, cool it with ice, filter the precipitated crystals, wash with 10 ml of ether, transfer it to the test tube, add 15 ml of ether, heat it in a warm water bath to dissolve, pour out the ether solution while it is hot, and evaporate Disperse ether to obtain white crystals (recrystallize once if necessary). After drying, measure according to the melting point determination procedure. The melting point is 120~125°C.
4.4.3. Identification
4.4.3.1. Take 1ml of the saturated aqueous solution of this product, add 0.5ml each of ferric chloride test solution and sodium hydroxide solution to form a brown color. The yellow precipitate does not disappear after shaking; when excess sodium hydroxide test solution is added dropwise, it dissolves into a brown solution.
4.4.3.2. The infrared light absorption spectrum of this product should be consistent with the control spectrum (spectrum set 84).
4.4.4. Inspection:
4.4.4.1. Acidity: Take 5.0g of this product, add 50ml of newly boiled cold water to dissolve, add 3 drops of phenolphthalein indicator solution and hydroxide Sodium titrant (0.02mol/L) 0.30ml, should be pink.
4.4.4.2. Clarity and color of the solution. Take 1.5g of this product and add 10ml of water to dissolve it. The solution should be clear and colorless; if it is turbid, it should not be darker than the No. 1 turbidity standard solution.
4.4.4.3. Chloride: Take 1.0g of this product and compare it with the control solution made of 3.0ml of standard sodium chloride solution according to the chloride inspection procedures. It should not be more concentrated (0.003).
4.4.4.4. Sulfate: Take 2.0g of this product and compare it with the control solution made from 2.0ml of standard potassium sulfate solution according to the sulfate inspection procedures. It should not be more concentrated (0.01).
4.4.4.5. Oxalate: Take 1.0g of this product, add 6ml of water, heat to dissolve, let cool, add 3 drops of ammonia test solution and 1ml of calcium chloride test solution, shake well, and place in a water bath After heating for 15 minutes, take it out and let it cool; if turbidity occurs, mix it with sodium oxalate solution (take 0.1523g of sodium oxalate, put it in a 1000ml measuring bottle, add water to dissolve and dilute to the mark, shake well. Each 1ml is equivalent to 0.1mg of oxalate (C2O4)) 2.0ml shall not be more concentrated (0.02) than the control solution prepared by the same method.
4.4.4.6. Loss on drying: Take this product and dry it to constant weight at 105℃. The weight loss should not exceed 0.5. Check according to the weight loss on drying inspection procedures.
4.4.4.7. The ignition residue shall not exceed 0.1 and shall be inspected according to the ignition residue inspection procedures.
4.4.4.8. For heavy metals, take 2.0g of this product, add 23ml of water to dissolve, then add 2ml of acetate buffer (PH3.5), and check according to the heavy metal inspection regulations. The heavy metal content should not exceed parts per million. ten.
4.4.4.9. For arsenic salt, take 1.0g of this product, add 10ml of water to dissolve it, add 5ml of dilute sulfuric acid and 0.5ml of potassium bromide bromine test solution, place it on a water bath and heat it for about 20 minutes to keep it slightly excessive. The presence of bromine (potassium bromide bromine test solution can be added dropwise if necessary), and the evaporated water should be replenished at any time, let cool, add 5ml of hydrochloric acid and an appropriate amount of water to make 28ml, check according to the arsenic salt inspection procedures, it should comply with the regulations (0.0002) .
4.4.5. Content determination
4.4.5.1. Operation: Take 0.2g of this product, weigh it accurately, place it in a 250ml measuring bottle, add water to dissolve and dilute to the mark. Shake well; accurately measure 10ml, place it in an iodine bottle, accurately add sodium periodate (potassium) solution (take 90ml of sulfuric acid solution (1→20) and 110ml of sodium periodate (potassium) solution (2.3→1000) to prepare into) 50ml, place on a water bath and heat for 15 minutes. Let cool, add 10 ml of potassium iodide test solution, seal tightly, leave for 5 minutes, titrate with sodium thiosulfate titrant (0.05 mol/L), when near the end point, add 1 ml of starch indicator solution, continue titration until the blue color disappears, and The titration results are corrected with a blank test. Each 1ml of sodium thiosulfate titrant (0.05mol/L) is equivalent to 0.9109mg of C6H14NO6.
4.4.5.2. Operating principle: A quantitative redox reaction occurs between mannitol and periodic acid. The remaining periodic acid and the generated iodic acid react with potassium iodide to generate free iodine. Use sodium thiosulfate to liquid titration.
Calculation formula: M (V sample - V empty) × 0.0009109
C6H14O6 = ×100
10
m× × 0.05
250
In the formula: M: molar concentration of Na2S2O3, mol/L;
V sample: volume of Na2S2O3 consumed by the sample, mL;
p>
V empty: the volume of Na2S2O3 consumed by the blank, mL;
m: sample mass, g.
4.4.5.4. Judgment criteria: Calculated based on dry product, the C6H14O6 content should be 98.0~102.0.
4.4.5.5. Allowable error: the relative deviation shall not exceed 0.5.
4.4.5.6. Operation precautions:
4.4.5.6.1. The pipette and volumetric flask used must be calibrated.
4.4.5.6.2. Pay attention to small bubbles when inhaling sodium periodate.
4.4.5.6.3. After adding potassium iodide, seal it tightly and add water to seal it.
4.4.5.6.4. Shake slightly slowly at the beginning of the titration, and gradually increase the speed; the dripping speed will be faster at the beginning, and slower when it is almost bright yellow. Add the starch indicator solution after it reaches bright yellow.
4.4.5.6.5. Freshly prepared starch indicator solution should be cooled to room temperature and should be used for no more than 1 week.
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