壹捌零玖壹捌柒(qi)肆(si)貮玖捌
來(lai)源:四部 分(fen)類:藥用輔料
Erjiajiyafeng Dimethyl Sulfoxide
C2H6OS 78.13 [67-68-5]
本品(pin)可由(you)二甲硫醚在氧化(hua)氮存(cun)在下(xia)通(tong)過(guo)空氣氧化(hua)制得(de);也可以(yi)從制造紙漿的副產(chan)物中制得(de)。
本品按無水物計算,應不得少于99.5%。
【性狀】本品為(wei)無色液體(ti);無臭或幾乎無臭;有引濕性。
本品與(yu)水、或乙m能任意(yi)混溶(rong),在烷烴中不溶(rong)。
凝點(dian) 本品的(de)凝點(dian)(通則0613)為17.0~18.3℃。
折(zhe)光率 本品的折(zhe)光率(通則0622)為1.478~1.479。
相對密度 本品的相對密度(通則0601)為(wei)1.095~1.105。
【鑒別】(1)取(qu)本品(pin)5ml,置(zhi)試管(guan)中(zhong),加氯(lv)化鎳50mg,振搖使溶(rong)(rong)(rong)解,溶(rong)(rong)(rong)液(ye)(ye)呈(cheng)(cheng)黃綠(lv)(lv)色(se),置(zhi)50℃水浴中(zhong)加熱,溶(rong)(rong)(rong)液(ye)(ye)呈(cheng)(cheng)綠(lv)(lv)色(se)或藍綠(lv)(lv)色(se),放冷,溶(rong)(rong)(rong)液(ye)(ye)呈(cheng)(cheng)黃綠(lv)(lv)色(se)。
(2)本品(pin)的紅外光吸收圖譜應與對照品(pin)的圖譜一致(通(tong)則0402)。
【檢查】酸度 取本(ben)品50.0g,加水100ml溶解后,加酚酞(tai)指示液0.1ml,用滴(di)定(ding)液(0.01mol/L)滴(di)定(ding)至溶液顯粉紅色(se),消耗滴(di)定(ding)液(0.01mol/L)不(bu)得過(guo)5.0ml。
吸(xi)(xi)光(guang)度(du)(du) 取本(ben)品(pin)適量,通(tong)人干燥氮氣15分鐘,以水(shui)為空(kong)白,照紫外-可見分光(guang)光(guang)度(du)(du)法(通(tong)則0401),立即測定,在(zai)275nm波(bo)長(chang)處的吸(xi)(xi)光(guang)度(du)(du)不(bu)得大于0.30;在(zai)285nm與(yu)295mn波(bo)長(chang)處的吸(xi)(xi)光(guang)度(du)(du)與(yu)275nm波(bo)長(chang)處的吸(xi)(xi)光(guang)度(du)(du)的比(bi)值,分別不(bu)得過0.65與(yu)0.45;在(zai)270~350nm的波(bo)長(chang)范圍(wei)內,不(bu)得有大吸(xi)(xi)收峰。
變深物 精密量取本品25ml,置(zhi)50ml量瓶中,加(jia)水(shui)0.5ml與1.0g,密塞,在(zai)水(shui)浴上加(jia)熱20分鐘,放冷,將溶液(ye)置(zhi)1cm吸(xi)收池中,以(yi)水(shui)為空(kong)白溶液(ye),照紫外-可見分光光度法(通則(ze)0401),在(zai)350nm的(de)波長處測(ce)定(ding)吸(xi)光度,不得大于(yu)0.023。
水(shui)(shui)分 取本品,照水(shui)(shui)分測定(ding)法(通則0832法1)測定(ding),含(han)水(shui)(shui)分不(bu)得過0.2%。
有(you)關物質(zhi) 取本(ben)品(pin)(pin),精(jing)密稱定(ding),用內(nei)標溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)(0.025%二(er)苯甲(jia)烷的丙酮(tong)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye))稀釋(shi)制成(cheng)(cheng)50%的溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye),作為(wei)供試(shi)(shi)(shi)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye);取供試(shi)(shi)(shi)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)適量,加(jia)內(nei)標溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)稀釋(shi)成(cheng)(cheng)0.050%的溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye),作為(wei)對照(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye);取二(er)甲(jia)基(ji)(ji)砜(feng)對照(zhao)品(pin)(pin)適量,精(jing)密稱定(ding),用上述內(nei)標溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)稀釋(shi)制成(cheng)(cheng)0.050%的溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye),作為(wei)二(er)甲(jia)基(ji)(ji)砜(feng)對照(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye);照(zhao)氣相(xiang)色(se)(se)譜法(通則0521)試(shi)(shi)(shi)驗,以10%聚乙二(er)醇20M為(wei)固定(ding)液(ye)(ye)(ye)(ye)(ye),柱溫為(wei)150℃,FID檢測(ce)器(qi);理(li)論板數按二(er)甲(jia)基(ji)(ji)砜(feng)峰(feng)計(ji)算(suan)不低于(yu)1500,二(er)甲(jia)基(ji)(ji)砜(feng)峰(feng)與內(nei)標峰(feng)的分離度應大于(yu)2.0。取供試(shi)(shi)(shi)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)、對照(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)、二(er)甲(jia)基(ji)(ji)砜(feng)對照(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)各2µl,分別注入氣相(xiang)色(se)(se)譜儀,記(ji)錄色(se)(se)譜圖。供試(shi)(shi)(shi)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)如顯二(er)甲(jia)基(ji)(ji)砜(feng)峰(feng),其(qi)與二(er)苯甲(jia)烷峰(feng)面(mian)積(ji)的比值,不得大于(yu)二(er)甲(jia)基(ji)(ji)砜(feng)對照(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)中二(er)甲(jia)基(ji)(ji)砜(feng)與二(er)苯甲(jia)烷峰(feng)面(mian)積(ji)的比值(0.1%)。供試(shi)(shi)(shi)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)中所有(you)雜質(zhi)峰(feng)面(mian)積(ji)總和(除主峰(feng)及(ji)內(nei)標峰(feng))與二(er)苯甲(jia)烷峰(feng)面(mian)積(ji)的比值不得大于(yu)對照(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(ye)中與二(er)苯甲(jia)烷峰(feng)面(mian)積(ji)的比值(0.1%)。
不(bu)揮發殘留物 取本(ben)品100g,精(jing)密稱定(ding),置105℃已干(gan)燥(zao)恒(heng)重(zhong)的蒸(zheng)發皿中,在通風櫥(chu)內置電(dian)熱板上緩(huan)緩(huan)蒸(zheng)發至(zhi)干(gan)(不(bu)發生沸騰(teng)),置105℃干(gan)燥(zao)3小時,稱重(zhong)。殘留物不(bu)得(de)過0.01%。
【含量(liang)(liang)測定】按(an)以(yi)下公式計算(suan)本品的含量(liang)(liang):
(1-不揮發殘留(liu)物-有(you)關物質)
含量= --------------------------------- ×
(1-水分)
【類別】藥用(yong)輔料,吸收(shou)促進劑、溶劑和防凍劑等(僅供外用(yong))。
【貯(zhu)藏】密閉,在陰(yin)涼、干燥處保存。
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