乙醇檢測在試劑和藥典中的應(yīng).ppt

乙醇檢測在試劑和藥典中的應(yīng)用,斯百全化學(xué)（上海）有限公司 Spectrum China Ltd. Spectrum質(zhì)檢部,800.720.5720,,乙醇,C2H6O 46.07 Ethanol. Ethyl alcohol CAS#: 64-17-5. 應(yīng)用： 飲料 汽車燃料 消毒劑 有機合成原料 溶劑 稀釋劑 萃取劑 洗滌劑,Spectrum 乙醇品種,A2176 Alcohol, Denatured, 190 Proof A1038 Alcohol, Anhydrous, Completely Denatured A1040 Reagent Alcohol, Denatured, Reagent, ACS E1020 Ethyl Alcohol, 190 Proof, FCC E1028 Ethyl Alcohol, Absolute, 200 Proof, Reagent, ACS E1029 Ethyl Alcohol, 190 Proof, Reagent, ACS E1068 Dehydrated Alcohol, 200 Proof, USP, EP, BP E1421 Alcohol, 190 Proof, BiotechGrade E1424 Dehydrated Alcohol, 200 Proof, BiotechGrade ET107 Dehydrated Alcohol, 200 Proof, Undenatured, USP ET108 Alcohol, 190 Proof, USP HP612 Reagent Alcohol, Denatured, Exceeds A.C.S. Specifications, HPLC Grade HS002 Reagent Alcohol, Denatured, Histological Grade EX0278 Alcohol, Denatured, OmniSolv(R) EX0289 Ethyl Alcohol, MultiPharm, 200 Proof, EP, JP, USP EX0290 Ethyl Alcohol, Pure, 190 Proof, HPLC Grade *Proof: 酒精純度, 一個酒精純度相當(dāng)于0.5的酒精含量.,E1028, Ethyl Alcohol, Absolute, 200 Proof, Reagent, ACS,TEST SPECIFICATION ASSAY (by VOLUME) 99.5 % - COLOR (APHA) 10 SOLUBILITY IN WATER TO PASS TEST WATER - 0.2 % RESIDUE AFTER EVAPORATION - 0.001 % ACETONE TO PASS TEST (limit about 0.001 %) ISOPROPYL ALCOHOL TO PASS TEST (limit about 0.003 %) TITRABLE ACID - 0.0005 meq/g TITRABLE BASE - 0.0002 meq/g METHANOL (CH3OH) - 0.1 % SUBSTANCES DARKENED BY (H2SO4) TO PASS TEST SUBSTANCES REDUCING PERMANGANATE TO PASS TEST,GB/T 678-2002 無水乙醇,A1040, Reagent Alcohol, Denatured, Reagent, ACS,TEST SPECIFICATION ASSAY: ETHANOL + METANOL (v/v) 94.0 - 96.0 % ISOPROPANOL (v/v) 4.0 - 6.0 % WATER - 0.5 % COLOR (APHA) 10 RESIDUE AFTER EVAPORATION - 0.001 %,HP612, Reagent Alcohol, Denatured, Exceeds A.C.S. Specifications, HPLC Grade,TEST SPECIFICATION ASSAY: ETHANOL + METANOL (v/v) 94.0 - 96.0 % ISOPROPYL ALCOHOL (v/v) 4.0 - 6.0 % ULTRAVIOLET ABSORBANCE (1 cm cell vs. water)- TO PASS TEST 205nm 1.00 210nm 0.65 220nm 0.35 230nm 0.20 250nm 0.04 270nm 0.01 300nm 0.005 COLOR (APHA) 10 RESIDUE AFTER EVAPORATION - 4 PPM WATER - 0.1 %,E1068, Dehydrated Alcohol, 200 Proof, USP, EP, BP,TEST SPECIFICATION ASSAY (by VOLUME) 99.5 % - CLARITY OF SOLUTION TO PASS TEST COLOR OF SOLUTION TO PASS TEST ACIDITY OR ALKALINITY TO PASS TEST RELATIVE DENSITY 0.790 - 0.793 SPECIFIC GRAVITY 15.56oC - 0.7962 UV ABSORPTION TO PASS TEST VOLATILE IMPURITIES TO PASS TEST NONVOLATILE RESIDUE TO PASS TEST IDENTIFICATION TO PASS TEST RESIDUAL SOLVENTS TO PASS TEST,乙醇含量檢測的應(yīng)用,相對密度法 USP, Specific Gravity. ET107, Dehydrated alcohol, 200 proof, undenatured, USP 蒸餾法 USP , Method . 中國藥典2005版一部：附錄 M 乙醇量測定法a, b, c 氣相色譜法 （GC） USP , Alcohol determination, Method . BE115, Belladonna Tincture ACS 10th, Ethyl alcohol. HP612，Reagent Alcohol, Denatured, Exceeds A.C.S. Specifications, HPLC Grade USP , Residual solvents, class 3. 中國藥典2010版二部：附錄 E 乙醇量測定法 中國藥典2005版一部：附錄 M 乙醇量測定法,相對密度法 - USP, Specific Gravity, method ET107, Dehydrated alcohol, 200 proof, undenatured, USP,Alcohol content: 99.2%, by weight; 99.5%, by volume, at 15.56. 原理: 25下, 相同體積乙醇和水的重量比值, 折算成15.56下乙醇的重量含量或體積含量. 方法: 使用同一比重瓶，先將先將一定體積的燒開過的蒸餾水放入其中, 分別稱量25 下空瓶和水裝入后的總重量, 兩者之差就是25 下水的重量. 同理測量 25 下乙醇的重量. 乙醇和水的重量比為25 下乙醇的比重. 通過查找USP reference table Alcoholometric table中的數(shù)據(jù)，確定15.56下乙醇的體積含量或者重量含量.,比重瓶,USP reference table Alcoholometric table,蒸餾法 - USP , Method 中國藥典2005版一部：附錄 M 乙醇量測定法,適用范圍 USP , Method : 流浸膏劑,酊劑 中國藥典2005版一部：附錄 M 乙醇量測定法: 流浸膏劑,酊劑,中藥制劑 原理 根據(jù)樣品的不同性質(zhì), 加入不同物質(zhì), 進行預(yù)處理. 蒸餾, 獲得乙醇餾出物. 測定蒸餾物的相對密度, 折算出乙醇的含量. 方法 (中國藥典2005版一部：附錄 M 乙醇量測定法) Alcohol content30%: 稱取20下樣品25ml, 置于150-200ml蒸餾瓶中, 加水約25ml, 蒸餾. 待餾出物達23ml時, 停止蒸餾. 加水至刻度, 測量乙醇在20下的相對密度, 計算出乙醇含量; Alcohol content30%: 稱取20下樣品25ml, 置于150-200ml蒸餾瓶中, 加水約50ml, 蒸餾. 待餾出物達48ml時, 停止蒸餾. 加水至刻度, 測量乙醇在20下的相對密度, 計算出乙醇含量; 樣品含有揮發(fā)性物質(zhì), 如揮發(fā)油, 三氯甲烷, 乙醚,樟腦等. 可先加入氯化鈉使之飽和, 后加入乙醚, 使溶液分層, 取水層按常規(guī)檢測. 樣品含有游離氨或揮發(fā)性酸. 可先加入稀硫酸或氫氧化鈉溶液, 調(diào)節(jié)酸堿度, 再按常規(guī)檢測.,蒸餾法 - USP , Method B1068, Benzalkonium Chloride Solution, 50 Percent, NF,Alcohol content10.0% 25下量取樣品25.0ml, 加水100ml, 365下蒸餾. 餾出物大約23ml時, 停止蒸餾, 在25下定容到25ml. 因餾出物渾濁, 加入CaCO3振搖, 過濾. 使用10ml比重瓶測量25下乙醇比重, 折算出乙醇含量. 結(jié)果: 乙醇餾出物比重 25 : 0.9938 乙醇含量: 4.2%,氣象色譜法 (GC) - ACS 10th: Ethyl Alcohol. HP612, Reagent Alcohol, Denatured, Exceeds A.C.S. Specification, HPLC Grade Specifications, HPLC Grade,Application: Ethyl Alcohol content 95.0% GC method Column: methyl silicone capillary Column temperature: 40 for 5 min, programmed to 220 at 10 /min, hold 2 min Injector temperature: 150-220 Detector temperature: 250 Sample size: 0.2 l splitless Carrier gas: helium at 3 ml/min Detector: TCD Measure the area under all peaks, and calculate the ethyl alcohol content in area percent,HP612, Reagent Alcohol, Denatured, Exceeds A.C.S. Specification, HPLC Grade Specifications, HPLC Grade,氣相色譜法 (GC) - USP , Alcohol determination, Method a. BE115, Belladonna Tincture,Application: Alcohol content: 65.0% - 70.0%. Column: DB-624 Column temperature: 120, Injector temperature: 210 Detector temperature: 210 Sample size: 5 l Carrier gas: nitrogen or helium Detector: FID Standard solution: 5ml each USP Alcohol RS and USP acetone RS together diluted by water to 50ml. Test stock solution: Dilute sample stepwise to get a 2% alcohol solution. Test solution: 5ml each test stock solution and USP acetone RS together diluted by water to 50ml. System Suitability Test: R2 (alcohol to acetone) tailing factor: 2.0 (alcohol) RSD2.0% (ratio of alcohol to acetone),BE115, Belladonna Tincture, Alcohol Content,氣相色譜法 (GC) - USP Residual Solvents,Application: Alcohol content: 5000ppm. Column: DB-624 Column temperature: 40 for 20 min, programmed to 240 at 10/min, hold 20 min Injector temperature: 140 Detector temperature: 250 Sample size: 5 ml, headspace Carrier gas: helium Detector: FID Split ratio: 5:1 System Suitability Test: R1.0 RSD2.0%,SU124, Sulfacetamide Sodium, Monohydrate, USP, Residual Solvents - Ethanol,中國藥典2005版一部：附錄 M 乙醇量測定法,適用范圍： 測定制劑中在20時乙醇的含量（%，ml/ml） 色譜條件與系統(tǒng)適應(yīng)性試驗：用鍵合交聯(lián)聚乙二醇為固定液的毛細管柱；起始溫度為50 ，維持7分鐘，再以每分鐘10 的速率升溫至110 ；進樣口溫度190 ；FID檢測器溫度220 。理論板數(shù)按正丙醇峰計算應(yīng)不低于8000，乙醇峰與正丙醇峰的分離度應(yīng)大于2.0. 校正因子測定：精密量取恒溫至20 的無水乙醇4ml、5ml、6ml，分別置100ml量瓶中，分別精密加入恒溫至20 的正丙醇（內(nèi)標(biāo)物質(zhì)）5ml，用水稀釋至刻度，搖勻，精密量取上述各溶液1ml，分別置100ml量瓶中，用水稀釋至刻度，搖勻（必要時可進一步稀釋），作為對照品溶液。取上述三種溶液各適量，注入氣相色譜儀，分別連續(xù)進樣3次，測定峰面積，計算校正因子，所得校正因子的相對標(biāo)準(zhǔn)偏差不得大于2.0%。 測定法：精密量取恒溫至20 的供試品適量（相當(dāng)于乙醇約5ml），置100ml量瓶中，精密加入恒溫至20 的正丙醇5ml，用水稀釋至刻度，搖勻，精密量取該溶液1ml，置100ml量瓶中，用水稀釋至刻度，搖勻（必要時可進一步稀釋），作為供試品溶液。取1l注入氣相色譜儀，測定，即得。,CNAS T0546 能力驗證 氣相色譜法測定藥品中乙醇含量,樣品名稱: T1064盲樣 方法: 中國藥典2005版一部：附錄 M 乙醇量測定法;或?qū)嶒炇页Ｓ脷庀笊V法 能力驗證結(jié)果 實驗結(jié)果: 47.92% 平均值: 46.39% Z絕對值: 7.123, 不合格結(jié)果 復(fù)測結(jié)果 實驗結(jié)果: 46.23% 平均值: 46.39% Z絕對值: 0.21, 滿意結(jié)果,原因分析,CNAS T0546 能力驗證 氣相色譜法測定藥品中乙醇含量 直接進樣,CNAS T0546 能力驗證 氣相色譜法測定藥品中乙醇含量 頂空進樣,CNAS T0546 能力驗證 氣相色譜法測定藥品中乙醇含量 頂空進樣,總結(jié),方法偏離和確認(rèn) 方法驗證 精密度 準(zhǔn)確度 專屬性 線性 儀器比對 人員比對 方法比對 實驗室間比對,小知識：Alcohol, Aldehyde-free 無醛乙醇的制備,USP - Dissolve 2.5 g of lead acetate in 5 mL of water, add the solution to 1000 mL of alcohol contained in a glass-stoppered bottle, and mix. Dissolve 5 g of potassium hydroxide in 25 mL of warm alcohol, cool the solution, and add it slowly, without stirring, to the alcohol solution of lead acetate. After 1 hour shake the mixture vigorously, allow it to stand overnight, decant the clear liquid, and recover the alcohol by distillation. 溶解2.5g醋酸鉛于5ml水中，將溶液加到裝有1000ml乙醇的具塞玻璃瓶中，混合。溶解5g氫氧化鉀于25ml溫的乙醇中，冷卻，將此溶液緩慢地加到醋酸鉛的乙醇溶液中，不用攪拌。1小時后，劇烈振蕩該混合液，放置過夜，輕輕倒出澄清液體，蒸餾，得到無醛乙醇。 EP - Mix 1200 ml of ethanol (96%) with 5 ml of a 40% w/v solution of silver nitrate and 10 ml of a cooled 50% w/v solution of potassium hydroxide . Shake, allow to stand for a few days and filter. Distil the filtrate immediately before use. 將1200ml乙醇和5ml的40%的硝酸銀溶液，以及10ml的冷卻的50%的氫氧化鉀溶液混合。振蕩，放置數(shù)天后過濾。使用前蒸餾濾液，得到無醛乙醇。,小知識：Alcohol, Neutralized中性乙醇的制備,USPTo a suitable quantity of alcohol add 2 or 3 drops of phenolphthalein TS and just sufficient 0.02 N or 0.1 N sodium hydroxide to produce a faint pink color. Prepare neutralized alcohol just prior to use. 一定量的乙醇中，加入2-3滴酚酞指示液，滴加0.02N或0.1N的氫氧化鈉溶液至溶液呈粉紅色。在使用前將乙醇調(diào)成中性即可。,小知識