第21卷第3期沈陽藥科大學(xué)學(xué)報(bào)Vol.21No.32004年5月Journal of Shenyang Pharmaceutical UniversityMay 2004 p. 190文章編號(hào): 1006 - 28582004 )3 - 0190- 03鋁鎂加的合成楊波',王國(guó)清2，吳英綿' ,伍百奇1 ,李瑞珍1(1.石家莊職業(yè)技術(shù)學(xué)院化工系河北石家莊050081 ; 2.沈陽藥科大學(xué)制藥系遼寧沈陽110016)摘要:目的研制新型抗酸藥鋁鎂加的合成方法。方法采用簡(jiǎn)單易行的溶液反應(yīng)合成鋁鎂加并運(yùn)用正交設(shè)計(jì)法優(yōu)化了合成工藝。結(jié)果對(duì)合成的鎂加鋁進(jìn)行了紅外光譜分析、差熱分析、熱重分析及X-射線粉末衍射分析確證了合成品結(jié)構(gòu)。結(jié)論該方法工藝簡(jiǎn)單易于工業(yè)化生產(chǎn)。關(guān)鍵詞:抗酸藥;鋁鎂加;正交設(shè)計(jì)法中圖分類號(hào):R 923.文獻(xiàn)標(biāo)識(shí)碼:A當(dāng)前抗酸藥的研究已從單-的含鋁或鎂的入CO2 ,100C反應(yīng)12 ho該方法操作復(fù)雜。鹽向羥基鋁鎂的復(fù)合物過渡,以提高抗酸效果及作者自擬方法:減少不良反應(yīng)1。鋁鎂加( almagate),分子式為硫酸鋁、硫酸鎂和碳酸鈉以-定濃度及摩爾AlMgd OH)( CO3); 4H2O2] ,由西班牙Amirail配比關(guān)系在-定條件下發(fā)生共沉淀置換反應(yīng)制研究所研制是一種中和作用迅速,中和能力強(qiáng)備。大作用持久無酸反彈現(xiàn)象吸附膽酸制酸活性原理:A2( sO4》+ 6MgSO, + 9Na2CO3 +不隨消化酶(特別是胃蛋白酶)作用而降低,不良11H2O- > Al2Mg6( OH )4( CO,》.4H2O +反應(yīng)小安全性高的新型抗酸劑。作者合成了鋁9Na,SO4+ 7CO2↑。鎂加并運(yùn)用光譜分析法確證了其結(jié)構(gòu)對(duì)其穩(wěn)定碳酸鈉水解出氫氧根并與鎂鹽、鋁鹽發(fā)生共.性進(jìn)行了考察。沉淀置換反應(yīng)生成鋁鎂加。1儀器與試藥在90C水浴電動(dòng)攪拌條件下將硫酸鋁、硫pHS- -3C 酸度計(jì)(上海第二分析儀器廠)多酸鎂適量配比的混合液及- -定量無水碳酸鈉的溶功能電子恒溫水浴鍋(.上海凱樂電子設(shè)備廠)精液同時(shí)緩慢滴加于適量水中約滴加1 h再繼續(xù)密電動(dòng)攪拌器( 100W廣州富城儀器廠) ,Brucker反應(yīng)20 min.將產(chǎn)物陳化后過濾蒸餾水充分洗IS- -55 紅外分光光度計(jì)( KBr壓片)熱重分析儀滌后,100C干燥即得。2.2鋁鎂加合成影響因素考察(杜邦公司,V5. 1A、Dupont 2000、General V4. 1C、Dupont 2100，吹掃氣:空氣,升溫速度:按照鋁鎂加含AlLO3為16.18%(理論值),10C min-1 升溫范圍:室溫~ 800C ) ,D/MAX-MgO為38.39%(理論值)，制酸力為rA轉(zhuǎn)旋陽極X_射線衍射儀(CuKa,50kV，28.60mEq g (理論值),考察合成中各因素水60mA石墨濾波)平變化對(duì)所得產(chǎn)品各種指標(biāo)的影響規(guī)律。通過大所用試劑皆為分析純,鋁鎂加(自制,批號(hào).量單因素實(shí)驗(yàn),確定了加料方式鋁、鎂鹽的投料001025 ) ,鋁鎂加Aldrine" (對(duì)照品揚(yáng)州一洋制藥配比無水碳酸鈉的用量是重要影響因素及其可有限公司)變動(dòng)的范圍。2.3鋁鎂加合成條件的正交設(shè)計(jì)優(yōu)化2實(shí)驗(yàn)部分中國(guó)煤化工見定前提下,以產(chǎn)品產(chǎn)2.1 鋁鎂加的合成.MYTHCNMHG選用L1d40 )正交表文獻(xiàn)3報(bào)道方法是:得16組合成條件。因素水平表(固定鎂鹽向Mg(OH)、A(OH)有機(jī)氨混合液中通63.5g)見表1結(jié)果見表2。收稿日期2003-11- 06作者簡(jiǎn)仿數(shù)鷯1976- )女漢族),遼寧昌圖人,助教碩士,主要從事藥學(xué)教育工作,Tel (0311 )3616611 - 8093 ,E - mail yb76s@ yahoo. com. cn。第3期楊波等鋁鎂加的合成191Table 1 The synthesis factors and the levels由直觀分析法對(duì)正交實(shí)驗(yàn)結(jié)果的分析可見,Levels硫酸鋁用量是影響產(chǎn)量的最主要因素。其4水平Factors3(30g )為最佳水平。Na2CO3用量是次重要的因mA(90,) 18H:o/g2:2829305052素其3水平最佳( 52g)反應(yīng)溫度對(duì)產(chǎn)量的影t/C90100 .110120響最小所以宜選擇1水平( 90C )Table 2 The results of different conditionsNo.mA(S04) 18H20gmNecao./gmyidd/g127.5( 1)50(1)90(1)20.6227.5( 1 )51(2)100(2)21.052( 3)110(3)20.8427.5(1)53(4)120(4)22.6528.5(2)50(1 )20.9651(2 )22.9752(3)23.98110( 3)21.9929.5( 3)23.01029.5(3)22.01222.71330.5( 4)120(4 )22.21430.5(4)24.11524.31653(4 )90( 1)23. 9Sk185.086.7090.40Sk289.690.0088.902k390.7092.0089.80》k494.5090.20k22 .2521.6822.6022 .4022. 5022.23k322 .6823. .0022.453.6322. 5522.509.505.30 .1.802.4鋁鎂加的結(jié)構(gòu)確證光譜、X射線粉末衍射光譜并分別進(jìn)行了熱分析。分別測(cè)定所合成的鋁鎂加及購(gòu)得的鋁鎂加2.4.1 紅外吸收光譜Aldrine* (對(duì)照品揚(yáng)州一洋制藥有限公司)的紅外紅外吸收光譜數(shù)據(jù)及解析歸屬見表3。，Table 3 Principal characteristic IR absorption of self-produced almagate and Aldrine"0σN0.20001025/ cmσAldrine' /cmσRerne data* / cmViberation form3 448.33 390.33400.一-OH H2O1 6251 602.3 .1 6301 4831 477.3中國(guó)煤化工1 4201 423.90O號(hào)一.1369.3.1 357.9 .Y8CNM HG1 110.41 119.3| 105* from Ref.[ 4]2.4.2 X射線粗末衍射圖譜的測(cè)定 與解析X-射線衍射圖譜數(shù)據(jù)對(duì)比見表4。192沈陽藥科大學(xué)學(xué)報(bào)第21卷Table 4 X-ray diffraction spectral data of self- produced almagate and Aldrine *No.001025Aldrine"Reference data。d/nmI:Io[:Io7.742 21007.728 77.616.477 226.421 1 .35.824 25.771 45.76284.211 04.462 44.015 364.164 23.8603473.8670503.813.316 53.3069.3.199 73.155 33.146 6.3.099 52.909 92.897082.89242.69622.689 92.583 02.580 22.57402.300 82.308 72.29522.210 9.2. 206752.15142.149 41.952 11.955 3131.941.741 6.1.741 61.73111.6440.1.617 91.527 6201.527 21.52351.498 2181.50271.419 24“Values from Ref.[ 4 ]由表4所列數(shù)據(jù)對(duì)比來看,自制鋁鎂加的X-二氧化碳。射線粉末衍射分析所得的面間距( d值)及衍射相3結(jié)果對(duì)強(qiáng)度比I:10 )值與對(duì)照品基本一致,且與文獻(xiàn)中鋁鎂加X射線粉末衍射所得主要數(shù)據(jù)吻合。首次采用簡(jiǎn)單易行的溶液反應(yīng)合成鋁鎂加運(yùn)2.4.3差熱分析( DTA )及熱重分析( TG)用正交設(shè)計(jì)法優(yōu)化了其合成工藝;與鋁鎂加測(cè)試結(jié)果顯示了2個(gè)吸熱峰,見圖1。Aldrine"對(duì)照品相比通過化學(xué)分析、IR光譜、X射線粉末衍射分析及熱分析結(jié)構(gòu)得到了確證。120-99.17%| 1727"C00-參考文獻(xiàn):391.67 °c-0.280[1]楊波，王國(guó)清.抗酸藥研究進(jìn)展[J ]沈陽藥科大學(xué)學(xué)0.1.報(bào)2001 18(2):148- 151.60F1[ 2 ] Moragues J ,Beneyto JE ,Fabragas JL ret al . Characteri-zation of a new crystalline synthetic gastric antacid- al-一 J-0.1200400600magate[ J ] Arneim-Forsch/Drug Res ,1984 ,34( II ):t/°C中國(guó)煤化工. The system MgO-Al2O3-Fig.1 DAT and TG profiles of almagateYHc N M H Gate and nitrate ions on the第1吸熱峰:177.27C。從100C ~phase equilibria[J]AmJ Sci ,1953 251 337- 361.177.27C樣品失重11.41%(理論值11.43% ) ,證[4 ]Fabregas JL ,Cucala J. Influence of microphysical struc-ture on in vitro activity of new synthetic antacids[ J ]明本品有4個(gè)結(jié)晶水存在。第2吸熱峰:Int J Pharm 1989 5x 2):173 - 178.391.67c.疵溫度為本品分解點(diǎn),放出結(jié)構(gòu)水及(下轉(zhuǎn)至第 214頁)214沈陽藥科大學(xué)學(xué)報(bào)第21卷Studies on the effects of the ligu capsules on pre-venting and treating the osteoporosisZHAO Ya-hong ,GONG Xian-feng ,LI Yan , WANG Min- wei( School of Pharmacy ,Shenyang Pharmaceutical University , Shenyang 110016 , China )Abstract : Objective To study the effective of ligu capsules ( traditional Chinese medicine ) in rats with os-teoporosis induced by retinoic acid. Method Osteoporosis model was established through treating withretinoic acid. Bone mineral density , bone bending strength , the level of Ca、P、Mg、Cu、Zn in serum andbone weight、bone length、bone diameter were measured. Results Femur bone mineral density , bone bend-ing strength ,the level of Ca、P、Mg in serum in ligu capsules groups were significantly increased than thosein model group. Compared with model group , level of serum- ALP and HOP/Cre were decreased ,while fe-mur weight、bone length、bone diameter were increased in ligu capsules groups. Conclusions The data indi-cated that ligu capsules could prevent and treat osteoporosis in model rats induced by retinoic acid.Key words : osteoporosis ; ligu capsules ; retinoic acid(上接第192頁)Study on the synthesis and the stability of almagateYANG Bo' , WANG Guo-qing2 , WU Ying-mian' , WU Bai-qi' ,LI Rui-zhen'( 1. Department of Chemical Engineering , Shijiazhuang Vocational Technology Institute , Shijjiazhuang050081 , China ; 2. School of Pharmaceutical Engineering , Shenyang Pharmaceutical University ,Shenyang 110016 , China )Abstract : Objective To study the synthesis of almagate. Methods Applying orthogonal design method ,thesynthetic conditions of method have been optimized. Results Through determination of IR spectum ,X-raydiffraction spectrum differetial thermal analysis ,the structure of the self-prepared almagate was elucidated.Conclusions The technics of this method is simple and the method may be used for industrial production.Key words : antacid ; almagate ; orthogonal design中國(guó)煤化工MHCNM HG