化学药中有效成分含量分析检测方案

Sodium Hydrogen Carbonate inStomach MedicinePharmaceutical 9.Example of measurement NTIC-99325 KMApplication Nole Acidbase titration by Automatic Potentiometric Titrator Standard Japanesepharmacopoeia codex15 1.Abstract Sodium hydrogen carbonate is used in antacid or other pharmaceuticals. Here， asample from commercially sold stomach medicine is titrated with 0.5mol/L sulfuricacid according to Japanese Pharmacopoeia codex 15. The contained sodium hydrogencarbonate is determined by the endpoint， which is the maximum inflexion point ontitration curve. 2.Reference 1).Japanese pharmacopoeia codex 15：Quantitative determination of Sodium hydrogen carbonate B.Cautions in measurement 1)Use water or solvent without carbon dioxide in it. Refrain from ambient carbondioxide which may affect chemical reaction during measurement. 2)Obtain the factor ofstandard 0.5mol/L sulfuric acid using carbon dioxideaccording to JIS K 8001. 3)Sodium hydrogen carbonate gradually dissolves in damp air. Handle with care. Http：//www. shxf17. com 4.Post-measurement care The electrode after rinsed with pure water must be kept in pure water in a beaker sothat its tip may not dry up. 5.Test equipment Main unit ： Automatic potentiometric titrator (Standard preamplifier： STD-) Electrode ： Combination glass electrode C-172 LN 98100C172」optional Temperature compensation electrode T-111[N 98100T111] optional 6.Reagent Reagent：：0.5mo1/L sulfuric acid 7.Measurement procedure ·Measurement- 1)Prepare approximately 2g of sample in a 200mL beaker. 2)Add pure water to make it total 100mL. 3))Titrate with 0.5mol/L sulfuric acid. 8.Formula Content(%)=(EP1一BL1)×TF×C1×K1/SIZE EP1 ：Titration volume (mL) BL1 Blank level (mL)=0 TF Factor =1.008 C1 ：Concentration conversion coefficient =84.01 (Sodium hydrogen carbonate (mg) equivalent to 1mL of 0.5mol/L H2SO4K1 Unit conversion coefficient=0.1 SIZE Sample size (g) 上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Http：//www.shxf17.com -Ambient condition-一 Room temperature ： 22.5℃ Humidity 47% Weather： Cloudy The below test data were obtained from titration by AT-510 unit. Sample No. ： 60-01Date： 1999/08/10 10：10Sample ID ：NaHCO3 Method No. ： 19 Method Name ： NaHCO3 Titr. Time ：00：10：45 Size ：1.960gConc-1 ：5.2084% End point-1 Volume ： 1.2055mLPotential： 5.45pH5.G · [pH] 6.00.033 8.008 [nL] -Titration parameter- Model ：AT-510 Method No. ： 19 Form ： EP Stop Calc. Type ： Sample APB No. ：1 Conc.1 ：Set Unit No. ：1 CO1= Detector No. ：1 (EP1-BL1)*TF*K1*C1/SIZ Unit ：pH E Max.Volume ： 8.0mL Wait Time ：(0s Unit ：% Direction ：FAuto EPNo. ：11 Temp.Comp.：Off C1(mg/mL) ：84.01 End PointNo. ： 1 K1 ：0.1 End sense ： Auto End Point Area： Off Separation ：(Off Factor ：1.008 Over Titr.Vol. ： C0mL Conc ：0.5 Gain ：3 Data samp.Pot.： 4.0mV Data samp.Vol.： 0.5mL Blank1 ：0.0 Stability ：(0.5mV/s Delay Time ：1s Limit Time ：30s Meaning of printout data： 《Titration parameter> Form： of titration/ APB No. the power burette used in titration / Unit No.：APB Unit File numberDetector No.： the detector used in titration / Max Volume： of titration/Wait Time： before titration starts Direction.： of titration 《Control parameter》 End Point No.： total EPs / End sense： EP direction /End Point Area： detection areaSeparation： of potential level /Over Titr.Vol.： over-titration volume / Gain： of detection signalData samp.Pot. potential changes of sampling detection signal / Data samp.Vol.： titration volume of sampling signalStability： level of EP stability / Delay Time： before stability check /Limit Time： for stability check 《Result parameter> Calc.Type of formula/ Conc.1： formula 1 / Unit： of results /EP No.for calculation /Temp.Comp.： of titration liquidC1(mg/mL)： concentration conversion coefficient /K1： unit conversion coeff./ Factor： of reagent Blank1 blank level 1 -Measurement resultsS- Statistics Sampleg Titration(mL) Content(%) Mean SD RSD 1.960 1.960 5.2101% 0.007% 0.136% 1.2055 1.2077 1.2045 5.2084 5.2179 5.2041 *The above results were obtained by 3 tests of the same sample. *Red underline shows the data from page 3/4. 10.Summary Sodium hydrogen carbonate is used in antacid for stomach ulcer or irritation. Sinceit gradually dissolves in damp air， it is necessary to check its concentration forquality control by way of titration. The sample measurement this time shows a good repeatability with 0.1% relativestandard deviation. Precise and reliable measurement is assured by the automated potentiometry.The analysis of sodium hydrogen carbonate in stomach medicine can be perfectlymade by any of the following titration systems made by Kyoto Electronics (KEM). 【AT-610】 【AT-510】 【AT-500N-1】 AwardedProductt ofSupremeTechnology from Kyoto City · Compact and cost performancemodel · Low cost and high performance ·Easy view with back light LCD ·Easy key entry by touch panel oflarge color LCD (8-inch wide) ·PC card expands data memory forconvenience and versatility. ·GLP/GMP conformed mode ·Simultaneous titration in parallel · Bothpotentiometricand KarlFischer moisture titration(coulometric"volumetric) can beperformed at a time. KeM KYOTO ELECTRONICS MANUFACTURING CO.，LTD. Overseas Division： Yamawaki Bldg 9F，4-8-21 Kudan-minami，Chiyoda-ku， Tokyo 102-0074 JAPAN Phone： +81-3-3239-7333， Fax： +81-3-3237-0537 Head Office： 56-2 Ninodan-cho，Shinden，Kisshoin，Minami-ku， Kyoto 601-8317 JAPAN Phone： +81-75-691-4122， Fax： +81-75-691-9961 URL： http：//www.kyoto-kem.com 上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Tel： 021-66581985，63172460 Fax： 021-66581986 周峰 13916388882 zhou-feng1027@163.com Tel： Fax： 周峰 zhou-feng comTIC-Ver. Tel： Fax： 周峰 zhou-feng comTIC-Ver.