Yansuan Xiaobojian

Berberine Hydrochloride

本品(pin)為5 ， 6 - 二(er)氫(qing)- 9 ， 1 0 - 二(er)甲氧(yang)苯并3 - 苯并二(er)氧(yang)戊環(huan)[ 5 6 - Q ] 喹嗪鹽酸鹽二(er)水合(he)物。按(an)無水物計算(suan)， 含Qo H 1 8 C 1 N 0 ， 提取品(pin)不(bu)(bu)得少于9 7 . 0% ， 合(he)成(cheng)品(pin)不(bu)(bu)得少于98. 0%

【性(xing)狀】本品為黃色結(jie)晶性(xing)粉末；無臭，味極(ji)苦。本品在(zai)熱水(shui)中溶解(jie)(jie)，在(zai)水(shui)或乙(yi)醇(chun)中微(wei)溶，在(zai)三(san)氯甲(jia)烷中極(ji)微(wei)溶解(jie)(jie)，在(zai)乙(yi)醚中不溶。

【鑒別】（ 1 ） 取本品約O . l g ，加水K J m l ，緩緩加熱溶(rong)解后，加氫氧化鈉試液(ye)4滴(di)，放(fang)冷（必要時(shi)濾過），加丙酮8滴(di)，即(ji)發生渾濁。

（2） 取本品(pin)約5 m g ，加(jia)(jia)稀鹽酸(suan)2ml ，攪拌，加(jia)(jia)漂白粉(fen)少(shao)量，即顯櫻(ying)紅色。

（3） 本品的紅外(wai)光(guang)吸收(shou)圖譜應與(yu)對照的圖譜（光(guang)譜集(ji)3 2 0圖）一致，U ） 取本品約0 . lg，加水20ml，緩緩加熱(re)溶解后，加硝酸0.5ml，冷卻，放置10分鐘，濾過(guo)，濾液顯氯化物(wu)的鑒別（1）反應（附錄in）。

【檢(jian)查】有關(guan)物質(zhi) 取(qu)本品(pin)(pin)適(shi)量(liang)(liang)，精密稱定，加(jia)流(liu)動(dong)相溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)解(jie)并定量(liang)(liang)稀(xi)釋制(zhi)成每l m l 中含(han)l m g 的(de)(de)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)， 作(zuo)為(wei)供試品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)；另取(qu)鹽酸藥(yao)根(gen)堿對(dui)(dui)照(zhao)(zhao)(zhao)品(pin)(pin)和鹽酸巴馬汀(ting)對(dui)(dui)照(zhao)(zhao)(zhao)品(pin)(pin)適(shi)量(liang)(liang)，精密稱定， 加(jia)流(liu)動(dong)相溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)解(jie)并定量(liang)(liang)稀(xi)釋制(zhi)成每l m l 中含(han)O . l m g 的(de)(de)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)，分別作(zuo)為(wei)對(dui)(dui)照(zhao)(zhao)(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)（1）和（2）;精密量(liang)(liang)取(qu)供試品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)2ml和對(dui)(dui)照(zhao)(zhao)(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)（1）和（2）各10ml，置100ml量(liang)(liang)瓶中，用(yong)流(liu)動(dong)相稀(xi)釋至(zhi)(zhi)刻度，搖勻，作(zuo)為(wei)對(dui)(dui)照(zhao)(zhao)(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)i取(qu)對(dui)(dui)照(zhao)(zhao)(zhao)品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)（2）1ml，用(yong)供試品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)稀(xi)釋至(zhi)(zhi)1 0 m l，搖勻，作(zuo)為(wei)系統適(shi)用(yong)性試驗溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)。照(zhao)(zhao)(zhao)高效液(ye)(ye)(ye)(ye)相色(se)(se)譜(pu)(pu)(pu)(pu)法(fa)（附錄V D ）試驗，用(yong)十(shi)八烷(wan)基硅(gui)烷(wan)鍵合(he)硅(gui)膠為(wei)填充(chong)劑；以0. O l m o l / L 磷酸二氫銨(an)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)（ 用(yong)磷酸調(diao)(diao)節p H 值至(zhi)(zhi)2.8）-乙腈（75 2 5 ）為(wei)流(liu)動(dong)相；檢(jian)測(ce)波長為(wei)3 4 5 n m。取(qu)系統適(shi)用(yong)性試驗溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)lOpl，注入液(ye)(ye)(ye)(ye)相色(se)(se)譜(pu)(pu)(pu)(pu)儀，巴馬汀(ting)峰(feng)(feng)與(yu)小檗(bo)堿峰(feng)(feng)間(jian)的(de)(de)分離(li)度應符合(he)要求。另取(qu)對(dui)(dui)照(zhao)(zhao)(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)l O f x l ， 注入液(ye)(ye)(ye)(ye)相色(se)(se)譜(pu)(pu)(pu)(pu)儀，調(diao)(diao)節檢(jian)測(ce)靈敏度，使小檗(bo)堿色(se)(se)譜(pu)(pu)(pu)(pu)峰(feng)(feng)的(de)(de)峰(feng)(feng)高約為(wei)滿量(liang)(liang)程的(de)(de)2 5 % 。精密量(liang)(liang)取(qu)對(dui)(dui)照(zhao)(zhao)(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)與(yu)供試品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)各1 0 p l ， 分別注入液(ye)(ye)(ye)(ye)相色(se)(se)譜(pu)(pu)(pu)(pu)儀， 記錄色(se)(se)譜(pu)(pu)(pu)(pu)圖(tu)至(zhi)(zhi)主成分色(se)(se)譜(pu)(pu)(pu)(pu)峰(feng)(feng)保(bao)留時(shi)(shi)間(jian)的(de)(de)2 倍。供試品(pin)(pin)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)的(de)(de)色(se)(se)譜(pu)(pu)(pu)(pu)圖(tu)中，如(ru)有與(yu)藥(yao)根(gen)堿峰(feng)(feng)和巴馬汀(ting)峰(feng)(feng)保(bao)留時(shi)(shi)間(jian)一(yi)致的(de)(de)色(se)(se)譜(pu)(pu)(pu)(pu)峰(feng)(feng)，按外標法(fa)以峰(feng)(feng)面(mian)積(ji)(ji)計算，均不得(de)過1.0%;其(qi)他雜(za)質(zhi)峰(feng)(feng)面(mian)積(ji)(ji)的(de)(de)和不得(de)大于對(dui)(dui)照(zhao)(zhao)(zhao)溶(rong)(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(ye)(ye)中小檗(bo)堿峰(feng)(feng)的(de)(de)峰(feng)(feng)面(mian)積(ji)(ji)（ 2 . 0 % ） 。

氰化物(wu) 取本(ben)品(pin)(pin)(pin)(pin)(pin)0 . 50g，依法檢(jian)查（附(fu)錄(lu)《 F第一法），應符合(he)規定(ding)(ding)（合(he)成(cheng)品(pin)(pin)(pin)(pin)(pin)）。有機(ji)腈(jing)(jing)取研細的本(ben)品(pin)(pin)(pin)(pin)(pin)約0 . 2 5 g，精(jing)密稱(cheng)定(ding)(ding)，置2 5 m l具塞(sai)錐形瓶中(zhong)，加無(wu)水(shui)(shui)乙(yi)鰱5ml ，振搖5分鐘，用垂熔漏斗（G5）濾過，用無(wu)水(shui)(shui)乙(yi)醚洗滌(di)3 4 2ml） 濾液(ye)(ye)(ye)與洗液(ye)(ye)(ye)，濃縮至約0 . 5 m l，作為供(gong)(gong)試(shi)品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)；另取胡椒乙(yi)腈(jing)(jing)對(dui)(dui)照品(pin)(pin)(pin)(pin)(pin)適量(liang)，精(jing)密稱(cheng)定(ding)(ding)， 加三氱甲烷溶(rong)(rong)(rong)解(jie)并稀釋制(zhi)成(cheng)每l m l 中(zhong)約含(han)0 . l m g的溶(rong)(rong)(rong)液(ye)(ye)(ye)，作為對(dui)(dui)照品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)。照薄(bo)(bo)層色(se)譜法（附(fu)錄(lu)V B）試(shi)驗(yan)，吸取對(dui)(dui)照品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)l O p l 與供(gong)(gong)試(shi)品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)全(quan)f l ，分別點(dian)于同一硅膠G（厚度0.5mm）薄(bo)(bo)層板(ban)上(shang)，以(yi)(yi)苯-冰醋酸(suan)（25 ： 0.1）為展(zhan)開劑，展(zhan)開，晾干，噴以(yi)(yi)5 %鉬(mu)酸(suan)銨硫酸(suan)溶(rong)(rong)(rong)液(ye)(ye)(ye)，在(zai)(zai)1 0 5 ° C加熱1 0 2 0鐘，檢(jian)視(shi)，供(gong)(gong)試(shi)品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)在(zai)(zai)與對(dui)(dui)照品(pin)(pin)(pin)(pin)(pin)溶(rong)(rong)(rong)液(ye)(ye)(ye)所顯主斑點(dian)的相應位置上(shang)，不(bu)得(de)顯雜質斑點(dian)（合(he)成(cheng)品(pin)(pin)(pin)(pin)(pin)）。

水分(fen) 取本(ben)品， 照(zhao)水分(fen)測(ce)定法(fa)（ 附錄M M 第一法(fa)A ） 測(ce)定，含(han)水分(fen)不得過(guo)12.0%

熾灼(zhuo)殘(can)渣(zha) 取 本 品(pin) l . O g ，依(yi)法檢査（附錄W N），遺留殘(can)渣(zha)不得過0 . 2%（提取品(pin)）或0. 1%（合成品(pin)）。

重金屬 取熾灼(zhuo)殘渣(zha)項下遺留的殘渣(zha)， 依法檢査(cha)（ 附錄? H第(di)二(er)法），含重金屬不得過百(bai)萬(wan)分(fen)之二(er)十（合成品）。

【含(han)量(liang)測定(ding)(ding)】取本品(pin)約0.3g，精密稱(cheng)定(ding)(ding)，置(zhi)(zhi)燒杯中，加(jia)沸水(shui)150ml使溶(rong)解(jie)，放冷，移置(zhi)(zhi)250ml量(liang)瓶(ping)中，精密加(jia)重格酸(suan)(suan)鉀(jia)滴(di)定(ding)(ding)液（0.016 67mol/L）50ml，加(jia)水(shui)稀(xi)釋至刻(ke)度(du)，振搖(yao)(yao)5分鐘(zhong)，用干燥濾(lv)紙濾(lv)過，精密量(liang)取續(xu)濾(lv)液1 0 0 m l ，置(zhi)(zhi)2 5 0 m l具(ju)塞(sai)錐形瓶(ping)中，加(jia)碘化鉀(jia)2g，振搖(yao)(yao)使溶(rong)解(jie)，加(jia)鹽(yan)酸(suan)(suan)溶(rong)液（1 — 2） 10ml，密塞(sai)，搖(yao)(yao)勻(yun)，在暗處(chu)放置(zhi)(zhi)10分鐘(zhong)，用硫代硫酸(suan)(suan)鈉滴(di)定(ding)(ding)液（0. lmol/L）滴(di)定(ding)(ding)，至近終點時，加(jia)淀粉指示液2 m l ， 繼(ji)續(xu)滴(di)定(ding)(ding)至藍色消失(shi)， 溶(rong)液顯亮(liang)綠色， 并將滴(di)定(ding)(ding)的結果用空A 試(shi)驗校正。每l m l重鉻酸(suan)(suan)鉀(jia)滴(di)定(ding)(ding)液（0 . 016 6 7 m o l / L ） 相當于(yu)1 2 . 3 9 m g 的C 2 。H 1 8 C 1 N 0 "