壹捌(ba)(ba)零(ling)玖壹捌(ba)(ba)柒肆貮玖捌(ba)(ba)
來源:四部(bu) 分類:藥用輔料
Erjiajiyafeng Dimethyl Sulfoxide
C2H6OS 78.13 [67-68-5]
本品(pin)可(ke)由二甲硫醚在氧化氮存在下通過空氣氧化制(zhi)得(de);也(ye)可(ke)以從(cong)制(zhi)造紙漿的(de)副產物中制(zhi)得(de)。
本品按無水物計算,應(ying)不得少于(yu)99.5%。
【性狀】本品為無色液體;無臭或幾(ji)乎無臭;有引濕性。
本品與水、或乙m能任意混溶,在烷(wan)烴中不溶。
凝(ning)點(dian) 本品的凝(ning)點(dian)(通則0613)為17.0~18.3℃。
折(zhe)光(guang)(guang)率 本品的(de)折(zhe)光(guang)(guang)率(通則0622)為1.478~1.479。
相對密(mi)度 本(ben)品的相對密(mi)度(通則0601)為1.095~1.105。
【鑒別】(1)取本品5ml,置試管中,加氯(lv)化鎳50mg,振(zhen)搖使(shi)溶(rong)解,溶(rong)液呈黃(huang)綠色(se),置50℃水(shui)浴中加熱,溶(rong)液呈綠色(se)或(huo)藍綠色(se),放冷,溶(rong)液呈黃(huang)綠色(se)。
(2)本(ben)品的(de)紅外光吸收(shou)圖譜應與(yu)對照品的(de)圖譜一致(通(tong)則0402)。
【檢(jian)查(cha)】酸度 取(qu)本品50.0g,加水(shui)100ml溶解后(hou),加酚酞指示液0.1ml,用滴(di)定液(0.01mol/L)滴(di)定至(zhi)溶液顯粉紅(hong)色,消(xiao)耗滴(di)定液(0.01mol/L)不得過5.0ml。
吸光(guang)(guang)度 取本品適(shi)量,通人干(gan)燥氮氣15分鐘(zhong),以(yi)水為空白,照紫外-可見分光(guang)(guang)光(guang)(guang)度法(通則0401),立即測定,在275nm波(bo)長(chang)處(chu)的吸光(guang)(guang)度不(bu)得(de)大于(yu)0.30;在285nm與(yu)295mn波(bo)長(chang)處(chu)的吸光(guang)(guang)度與(yu)275nm波(bo)長(chang)處(chu)的吸光(guang)(guang)度的比值,分別不(bu)得(de)過0.65與(yu)0.45;在270~350nm的波(bo)長(chang)范圍(wei)內,不(bu)得(de)有大吸收峰。
變(bian)深物 精密(mi)量取本品25ml,置50ml量瓶中(zhong),加(jia)水0.5ml與(yu)1.0g,密(mi)塞,在水浴上(shang)加(jia)熱(re)20分鐘,放冷,將溶液置1cm吸收池(chi)中(zhong),以水為空(kong)白溶液,照(zhao)紫外(wai)-可(ke)見(jian)分光(guang)光(guang)度法(通則0401),在350nm的波(bo)長處(chu)測定吸光(guang)度,不得(de)大于(yu)0.023。
水(shui)(shui)分 取本品(pin),照水(shui)(shui)分測定(ding)(ding)法(通則0832法1)測定(ding)(ding),含水(shui)(shui)分不(bu)得過0.2%。
有關物質 取(qu)本(ben)品(pin)(pin)(pin),精密稱定(ding),用內標(biao)(biao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)(0.025%二(er)(er)苯(ben)(ben)甲(jia)(jia)(jia)(jia)(jia)烷(wan)的(de)(de)(de)(de)(de)丙酮溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye))稀(xi)釋制(zhi)成50%的(de)(de)(de)(de)(de)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye),作(zuo)為(wei)(wei)(wei)供(gong)試(shi)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye);取(qu)供(gong)試(shi)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)適(shi)量(liang),加(jia)內標(biao)(biao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)稀(xi)釋成0.050%的(de)(de)(de)(de)(de)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye),作(zuo)為(wei)(wei)(wei)對(dui)照(zhao)(zhao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye);取(qu)二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)對(dui)照(zhao)(zhao)品(pin)(pin)(pin)適(shi)量(liang),精密稱定(ding),用上述內標(biao)(biao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)稀(xi)釋制(zhi)成0.050%的(de)(de)(de)(de)(de)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye),作(zuo)為(wei)(wei)(wei)二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)對(dui)照(zhao)(zhao)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye);照(zhao)(zhao)氣(qi)相(xiang)色(se)譜法(通則0521)試(shi)驗,以10%聚乙(yi)二(er)(er)醇20M為(wei)(wei)(wei)固定(ding)液(ye)(ye)(ye)(ye),柱(zhu)溫(wen)為(wei)(wei)(wei)150℃,FID檢測器(qi);理論板數按二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)峰(feng)(feng)(feng)計算不(bu)低于(yu)1500,二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)峰(feng)(feng)(feng)與(yu)內標(biao)(biao)峰(feng)(feng)(feng)的(de)(de)(de)(de)(de)分離度應(ying)大(da)于(yu)2.0。取(qu)供(gong)試(shi)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)、對(dui)照(zhao)(zhao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)、二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)對(dui)照(zhao)(zhao)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)各2µl,分別注(zhu)入氣(qi)相(xiang)色(se)譜儀(yi),記錄色(se)譜圖(tu)。供(gong)試(shi)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)如顯二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)峰(feng)(feng)(feng),其與(yu)二(er)(er)苯(ben)(ben)甲(jia)(jia)(jia)(jia)(jia)烷(wan)峰(feng)(feng)(feng)面(mian)積(ji)的(de)(de)(de)(de)(de)比值(zhi),不(bu)得大(da)于(yu)二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)對(dui)照(zhao)(zhao)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)中二(er)(er)甲(jia)(jia)(jia)(jia)(jia)基(ji)(ji)砜(feng)與(yu)二(er)(er)苯(ben)(ben)甲(jia)(jia)(jia)(jia)(jia)烷(wan)峰(feng)(feng)(feng)面(mian)積(ji)的(de)(de)(de)(de)(de)比值(zhi)(0.1%)。供(gong)試(shi)品(pin)(pin)(pin)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)中所有雜(za)質峰(feng)(feng)(feng)面(mian)積(ji)總和(he)(除(chu)主峰(feng)(feng)(feng)及(ji)內標(biao)(biao)峰(feng)(feng)(feng))與(yu)二(er)(er)苯(ben)(ben)甲(jia)(jia)(jia)(jia)(jia)烷(wan)峰(feng)(feng)(feng)面(mian)積(ji)的(de)(de)(de)(de)(de)比值(zhi)不(bu)得大(da)于(yu)對(dui)照(zhao)(zhao)溶(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)中與(yu)二(er)(er)苯(ben)(ben)甲(jia)(jia)(jia)(jia)(jia)烷(wan)峰(feng)(feng)(feng)面(mian)積(ji)的(de)(de)(de)(de)(de)比值(zhi)(0.1%)。
不(bu)揮發殘留(liu)物 取(qu)本品100g,精密稱定,置105℃已干燥恒重(zhong)的蒸發皿中,在通(tong)風櫥內置電熱板上(shang)緩緩蒸發至干(不(bu)發生沸騰),置105℃干燥3小時,稱重(zhong)。殘留(liu)物不(bu)得過0.01%。
【含(han)(han)量(liang)測定(ding)】按以下(xia)公式計(ji)算(suan)本品的含(han)(han)量(liang):
(1-不揮發(fa)殘留物(wu)-有(you)關物(wu)質)
含(han)量= --------------------------------- ×
(1-水(shui)分)
【類別】藥用(yong)輔(fu)料,吸收(shou)促進劑、溶(rong)劑和防凍劑等(僅供外用(yong))。
【貯藏(zang)】密閉,在(zai)陰(yin)涼、干燥處保存。
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