盐酸氯化硫胺素、盐酸盐、叶酸中水分含量检测方案(卡氏水分测定)

HITACHI日立Inspire the Next HIRANUMA APPLICATIONDATA Karl Fischer Titrator Data No. KF9 Water contents Drugs and Medicines-KF Coulometry Thiamine Chloride Hydrochloride andFolic Acid 1.Abstract Water contents of drugs and medicines could be determined by Karl Fischer coulometric titrator. In coulometric titration， iodine of Karl Fischerreagent is generated by electrolysis and generated iodine quantitatively reacts with water. Reaction formula is described below. When the moisture content is relatively high at the% level， the amount of sample added is as small as a few 10 mg. If the sample is in powder form，taking and adding samples with an “ultra-micro solid sampler”makes measurement easy and accurate. An example for water contents measurements ofthiamine chloride hydrochloride and folic acid performed by with ultra-micro solid sampler are introduced here. The measurement method wasdetermined with reference to Japanese Pharmacopeia. Reference 1) Japanese Pharmacopoeia Seventeenth Edition 2. Apparatus and Reagents (1)Apparatus Titrator ：Hiranuma Karl Fischer Coulometric titrator AQ-series Electrolytic cell(2)ReagentsAnode solutionCathode solution(3)Sampling tool ：Standard Cell without drain valve (P/N E324017-1) ：HYDRANAL Coulomat AG (Honeywell) ：HYDRANAL Coulomat CG (Honeywell) ：Ultra-micro solid sampler (P/N E730016-A， Fig.2.1) Fig.2.1 Ultra-micro solid sampler 3. Procedure Science for abetter tomorrow (1) Fill 100 mL of anode solution and one ampoule of cathode solution into the electrolytic cell as shown in Fig.3.1 . (2) Set the ultra-micro solid sampler on the lid of cell as shown in Fig.3.2. (3) Start blanking to attain stable background. (4) Take sample into the capsule and accurately weigh it. (5) Set the capsule on the sampler as pictured in the Fig.3.3. (6) Pull the plate of sampler to introduce capsule into the cell. (7) Start titration. Measurement parameter is shown in Table 4.1. (8) Set sample weight to sample size. Fig.3.1. Preparation of the reagents. Fig.3.2 Setting of ultra-micro solid sampler Fig.3.3. Introduction of sample. 4. Parameters and results Cal Mode 0：Sample weight(net) X=(H2O-BLANK)/SIZE Interval Time 30 sec Current MEDIUM S.Timer 10 min Blank Value 0 ug Unit Mode AUTO Auto Interval 0 g Minimum Count 5 ug Back Ground ON Sample Size Input Every Time Cell Type Standard Table 4.2. Results of water content measurement in drugs and medicines Sample Sample Water Water Statistics resul Remark Size (mg) (g) content (%) Thiamine Chloride 33.2 1005.4 3.0283 Avg. 3.0245% insoluble Hydrochloride 30.3 912.7 3.0122 SD 0.0109% 32.4 982.7 3.0330 RSD 0.4% Folic acid 12.5 814.9 7.8356 Avg. 7.7329% insoluble 15.0 962.9 7.7032 SD 0.0915 % 11.5 880.9 7.6600 RSD 1.2% 5.Note (1) Sampler， capsule and the other tools should be dried up well before use. (2) After adding 10 to 20 capsules to the cell， open the cell lid and remove the capsule. Capsules can be washed and reused. To measure 100 ug or less water detection， make sure stability of blanking. Low and stable background value is important factor for trace level (3) of water measurement. Keywords： KKarl Fischer， Coulometric titration， Pharmacopeia， Solid 热线电话：立科学仪器(北京)有限公司 这里介绍了一个使用超微固体采样器测量氯化硫胺盐酸盐和叶酸的水含量的案例。