滴定法与高效液相色谱法测定苦参提取液中苦参总碱含量比较研究

目的筛选苦参提取工艺研究中苦参总碱含量的测定方法。方法用滴定法和高效液相色谱(HPLC)法对苦参原药材、苦参醇提取液及酸水提取液中苦参总碱的含量测定进行对比研究。结果在测定苦参原药材、苦参醇提取液及酸水提取液中苦参总碱的含量时,滳定法所得的相对标准偏差(RSD)较HPLC法低(0.92%vs.6.30%、0.72%vs.8.85%、1.53%vs.4.00%)。结论在进行含苦参原药材的提取工艺研究时,宜采用滴定法对苦参总碱进行含量测定。     

穿心莲浸膏的提取工艺研究

目的对国家第一批非处方药穿心莲片中的浸膏进行提取工艺研究,探索含量高、成本低的提取方法.方法采用水提、水提醇沉、醇提、1%、0.5%、0.1%、0.04%、0.01%碳酸钠碱水(碱提酸沉法)等8种方法分别提取穿心莲浸膏,并用分光光度法测定主要有效成分穿心莲内酯含量,从材料、干浸膏得率和内酯含量几方面综合考虑进行比较.结果水提取虽然成本低,但干浸膏得率(20.00%)和内酯含量(6.33%)也很低.水提醇沉不仅得率(8.80%)最低,内酯含量(10.29%)也低,而且耗用乙醇、成本高.醇提内酯含量(41.74%)虽最高,但成本也高,且得率低.5种碱水(碱提酸沉法)提取比较,0.01%碱水提取的内酯含量(21.51%)最高,所用成本最低,含水量(0.75%)最低,平均回收率为96.88%.结论用万分之一碱水(碱提酸沉法)从穿心莲茎叶中提取穿心莲浸膏较为适宜.     

络合滴定法测定鞣柳硼三酸散中鞣酸含量

目的测定鞣柳硼三酸散中鞣酸的含量。方法采用锌滴定液测定鞣酸、乙二胺四乙酸二钠回滴过量锌离子的络合滴定法测定鞣酸的含量。结果精密度试验的RSD为0.34%（n=5）;平均回收率为99.56%,RSD=0.36%（n=9）。结论络合滴定法简便、快速、准确,可控制鞣柳硼三酸散中鞣酸的含量。     

醋柳黄酮中总黄酮及槲皮素、异鼠李素的含量测定

目的:建立醋柳黄酮(TFH)中的总黄酮、槲皮素和异鼠李素的含量测定方法.方法:利用分光光度法测定醋柳黄酮(TFH)中的总黄酮含量,利用RP-HPLC法分别测定醋柳黄酮中的槲皮素和异鼠李素的含量.结果:分光光度法测定总黄酮含量时,在2.12～10.60 mg·L-1(r=0.999 9)的浓度范围内线性关系良好,平均加样回收率为99.7%;RP-HPLC法测定槲皮素和异鼠李素时,槲皮素在1.032～4.644 mg·L-1(r=0.999 8)的浓度范围内、异鼠李素在1.941～8.735 mg·L-1(r=0.999 9)的浓度范围内线性关系良好,平均加样回收率槲皮素为99.5%,异鼠李素为101.9%.结论:方法简便准确,可用于醋柳黄酮的质量控制.     

甘露醇-旋光法测定鞣柳硼三酸散中硼酸的含量

目的建立旋光法测定鞣柳硼三酸散中硼酸的含量。方法以低浓度明胶溶液提取制剂中硼酸,利用甘露醇结合硼酸形成具有旋光性复合物,并建立鞣柳硼三酸散中硼酸的含量测定方法。结果硼酸浓度在5～20 g.L-1的浓度范围内与旋光度线性关系良好(r=0.999 2),方法的平均回收率为99.98%,RSD为1.3%。结论旋光法测定鞣柳硼三酸散中硼酸的含量,操作简便、快速,结果准确,重现性好。     

高效液相色谱法测定鞣柳硼三酸散中水杨酸的含量

目的:探讨用反相高效液相色谱法测定鞣柳硼三酸散中水杨酸的含量。方法:采用Symetry Shield RP18(5μm 4.6mm×250mm)Columm色谱柱;以0.05mol/L磷酸二氢钠缓冲液(pH2.6)-乙腈(50∶50)为流动相;检测波长233nm。结果:水杨酸在20.4～61.2μg/ml浓度范围内呈良好的线性关系,平均回收率为99.0%。结论:本法简便、准确、快速,适用于鞣柳硼三酸散中水杨酸的含量测定。     

丹参浸出物与灰分测定实验研究

目的　探索丹参浸出物测定方法 ,确定丹参浸出物及灰分检测指标 ,为制定丹参药材标准提供依据。方法　浸出物与灰分含量测定方法均采用《中华人民共和国药典》规定方法。结果　丹参药材浸出物含量测定结果 :冷水浸平均含量为 (5 8.3± 2 .5 ) %、热水浸平均含量为 (5 8.3± 2 .4 ) %、冷醇浸平均含量为(6 .5± 1.1) %、热醇浸平均含量为 (13.0± 1.2 ) %。灰分含量测定中得丹参药材总灰分平均含量为 (7.2 9±0 .86 ) %、酸不溶灰分平均含量为 (2 .4 6± 0 .4 3) % (置信区间均为 95 % )。结论　丹参药材浸出物测定宜选用冷水浸 ,其检测指标应为≥ 5 0 % ,总灰分检测指标应为≤ 9.5 % ,酸不溶灰分检测指标应为≤ 3.5 %。     

两色金鸡菊醇提物的质量标准研究

目的建立两色金鸡菊醇提物的质量标准。方法通过薄层色谱法(TLC)、水分测定、炽灼残渣测定、紫外分光光度法和高效液相色谱法对两色金鸡菊醇提物进行质量控制。结果薄层色谱显示供试品与对照品绿原酸斑点在相同的位置上显相同颜色,供试品鉴别分离出马里苷、黄酮奥卡宁和奥卡宁3个主要成分;两色金鸡菊醇提物的水分不得超过15%;炽灼残渣不得超过16%;两色金鸡菊醇提物中绿原酸含量(C_(16)H_(24)O_(12))不得少于0.8%;flavanomarein含量(C_(21)H_(22)O_(11))不得少于4%;marein含量(C_(21)H_(22)O_(11))不得少于8.5%;3,5-二咖啡酰基奎宁酸含量(C25H24O12)不得少于0.5%;总黄酮含量不得低于9%;总酚酸含量不得低于28.0%。结论根据《中国药典》中药质量标准研究制定技术要求建立了一套完整的两色金鸡菊醇提物质量标准。建立了TLC可定性鉴别两色金鸡菊醇提物中的各主要成分,通过一测多评法可定量控制两色金鸡菊醇提物中绿原酸、flavanomarein、marein和3,5-二咖啡酰基奎宁酸的含量,建立紫外分光光度法可测定两色金鸡菊醇提物中的总黄酮、总酚酸的含量。     

高效液相色谱法测定酮咯酸氨丁三醇注射液的含量

目的 :建立一种用高效液相色谱法测定酮咯酸氨丁三醇注射液含量的方法。方法 :采用HypersilODS2C185 μm柱 ,甲醇 水 冰醋酸 (5 5∶4 4∶1)为流动相 ,流速约为 1.2mL·min-1,检测波长为 2 4 9nm。结果 :该方法酮咯酸氨丁三醇含量线性范围为 0 .0 96～ 0 .336g·L-1,r =0 .9999,回收率为 99.38% ,RSD为 0 .4 2 % (n =6 )。结论 :该方法简便、准确 ,能满足制剂质量标准的要求。     

藏药秦艽花的质量标准提升研究

目的提升藏药秦艽花的质量标准,为全面评价其质量提供科学依据。方法采用显微及薄层色谱(TLC)法对16批不同产地、不同基原的秦艽花药材进行定性分析;参照2020年版《中国药典》(四部)通则中相应方法,分别进行水分、总灰分、酸不溶性灰分、醇溶性浸出物含量的测定;建立高效液相色谱(HPLC)法,同时测定秦艽花中5种成分(马钱苷酸、獐牙菜苦苷、龙胆苦苷、獐牙菜苷、异荭草苷)的含量。结果秦艽花药材粉末呈浅棕黄色;粉末显微特征清晰,可见花粉粒、导管、非腺毛、花冠表皮细胞和花萼表皮细胞等。TLC鉴别结果显示,在供试品色谱图中,与对照品(异荭草苷)色谱相应位置上显相同颜色的荧光斑点。16批药材的水分、总灰分、酸不溶性灰分、醇溶性浸出物的含量分别为5.40%~8.87%、3.76%~6.40%、0.27%~0.58%、26.81%~42.51%。含量测定方法学考察结果均符合药典要求;16批秦艽花样品中马钱苷酸、獐牙菜苦苷、龙胆苦苷、獐牙菜苷、异荭草苷的含量分别为3.13~9.36、1.26~22.39、13.80~74.60、1.24~12.22、2.58~14.96 mg/g。结论本研究在秦艽花已有质量标准的基础上增加了显微鉴别、TLC鉴别、含量测定以及水分、总灰分、酸不溶性灰分和醇溶性浸出物等检查项,并初步拟定秦艽花中水分不得过9.0%、总灰分不得过6.5%、酸不溶性灰分不得过0.6%、醇溶性浸出物不得少于26.0%、龙胆苦苷的含量不得低于13.8 mg/g。     

Decrease of gastrointestinal mucosal damage by salicyluric acid compared with salicylic acid in rabbits.

The gastrointestinal mucosal damage following the oral administration of salicylic acid or salicyluric acid was examined in rabbits using a scanning electron microscope. Six and 24 h after treatment with salicylic acid, morphological changes of gastric mucosa were recognized. In rabbits treated with salicyluric acid, however, severe damage in the gastric mucosa was not found after 24 h compared with the treatment with salicylic acid. Following the treatment with salicylic acid, some mucosal damage in the duodenum, jejunum and ileum was observed after 24 h. The surface character of the duodenal, jejunal, ileal, caecal and colonic mucosa were almost identical compared with the control following the treatment with salicyluric acid. It was reported that salicyluric acid is metabolized to salicylic acid by the intestinal microorganisms. From these results, it was suggested that prodrugs utilizing the metabolism of salicyluric acid to salicylic acid by intestinal microorganisms may be useful in reducing gastrointestinal mucosal damage.     

Preparation and evaluation of Eudragit gels. II: In vitro release of salicylic acid, sodium salicylate, and ketoprofen from Eudragit L and S organogels.

The in vitro dissolution characteristic of salicylic acid, sodium salicylate, and ketoprofen from Eudragit L and S organogels was investigated by the rotation disk method. The dissolution pattern of salicylic acid and erosion of Eudragit L polymer from the organogels followed apparent zero-order kinetics, providing strong evidence for a surface erosion mechanism and negligible diffusional release of salicylic acid. On the other hand, the dissolution of salicylic acid from Eudragit S organogels was a linear function of the square root of time. The apparent dissolution rate of salicylic acid from Eudragit S organogels increased with increasing temperature from 32 to 42 degrees C and agitation rate from 50 to 200 rpm. A linear relationship was obtained between the logarithm of apparent dissolution rate constants and the reciprocal of absolute temperatures. The activation energy for release of salicylic acid from Eudragit S organogels was in the range of 2.99 to 5.57 kcal/mol. From various experimental results, it was concluded that the release process of salicylic acid from Eudragit S organogels was diffusion controlled through the organogels matrix.     

HPLC法测定三种制剂中水杨酸的含量

目的：建立测定三种制剂（水杨酸软膏、水杨酸硫软膏、复方硫软膏）中水杨酸含量的方法。方法：采用HPLC法,色谱柱：Diamonsil C18（250 mm×4.6 mm,5μm）;流动相：甲醇-0.1 mol·L^-1磷酸二氢钠（30：70）;检测波长：231 nm;流速：1.0 mL·min^-1;柱温：35℃;进样量：10μL。结果：水杨酸与其它杂质峰分离良好,水杨酸在12.32-123.20μg·mL^-1范围内与峰面积呈良好的线性关系（r=1.000 0）;水杨酸在水杨酸软膏、水杨酸硫软膏、复方硫软膏的平均回收率分别为100.55%、99.96%、99.13%,RSD分别为0.95%（n=9）、0.96%（n=9）、1.15%（n=9）。结论：采用该方法测定三种制剂中的水杨酸含量,简便易行,结果准确,可作为三种制剂中水杨酸的质量控制方法。     

二阶导数光谱法同时测定双组分体系中阿司匹林和水杨酸的含量

目的：建立二阶导数紫外光谱法同时测定双组分体系中阿司匹林和水杨酸浓度。方法：配制阿司匹林和水杨酸的系列标准溶液,记录样品在230～350nm的紫外扫描图谱,并求二阶导数光谱;采用二阶导数光谱法和等吸收波长法分别测定混合物中阿司匹林和水杨酸的含量,计算回收率。结果：二阶导数光谱法测定双组分体系中阿司匹林的平均回收率为（100.32±0.94）%,水杨酸的平均回收率为（100.34±0.61）%;等吸收波长法能够准确测定混合体系中阿司匹林的含量,测定回收率为（99.66±1.17）%,但水杨酸测定误差较大,平均回收率为（104.16±3.65）%。结论：二阶导数光谱法操作简便,结果准确,可同时准确测定双组分体系中阿司匹林和水杨酸的含量。     

Carrier-Mediated Absorption of Salicylic Acid from Hamster Cheek Pouch Mucosa

Previously, we found that monocarboxylic acids undergo carrier‐mediated transport in primary cultures of oral mucosal epithelial cells.¹ In this study, we investigated whether carrier‐mediated absorption of a monocarboxylic acid from the oral mucosa occurs in vivo. Salicylic acid was administered to hamster cheek pouch. At predetermined intervals, the concentration of salicylic acid in the fluid remaining in the cheek pouch lumen and the blood salicylic acid concentration were determined. The absorption of salicylic acid was saturable at high salicylic acid concentrations. Sodium azide, a metabolic inhibitor, and carbonylcyanide p‐trifluoromethoxyphenylhy‐drazone (FCCP), a protonophore, significantly inhibited the absorption of salicylic acid but not the absorption of salicylamide from the oral mucosa. Various monocarboxylic acids inhibited the absorption of salicylic acid, whereas dicarboxylic acids had no such effect. Transfer of [¹⁴C]salicylic acid from the cheek pouch mucosa to the systemic circulation was observed, and the blood [¹⁴C]salicylic acid concentration in the case of coadministration with propionic acid was significantly lower than that in the case of no propionic acid coadministration. These results show that monocarboxylic acids undergo carrier‐mediated absorption from the hamster cheek pouch mucosa.     

水杨酸微乳的制备及质量评价

目的制备水杨酸微乳并进行质量评价。方法采用吐温-80作乳化剂,肉豆蔻异丙酯为油相,借助伪三元相图的研究手段确定乳化剂和助乳化剂的最佳配比,制成不同浓度的水杨酸微乳,并从含量测定、透光率、pH值、比重、黏度测定和稳定性方面进行了评价。结果吐温-80与1,2-丙二醇的配比为15：1,其微乳区最大,几种浓度的水杨酸制剂均能形成微乳且稳定分散于制剂中。结论微乳能增加水杨酸在制剂中的溶解度,方便于临床应用和提高了治疗效果。     

联立方程分光光度法测定复方苯甲酸醇溶液中两组分含量

目的建立复方苯甲酸醇溶液中苯甲酸和水杨酸的含量测定方法。方法采用联立方程分光光度法,直接测定复方苯甲酸醇溶液中苯甲酸和水杨酸的含量。结果以229nm和236nm分别为苯甲酸和水杨酸的测定波长,以0．1mol／L的盐酸为空白,苯甲酸质量浓度在2．535～17．745μg／mL,水杨酸质量浓度在1．265～8．855μg／mL范围内与吸收度线性关系良好,平均回收率分别为99．08％和98．70％,RSD分别为0．93％和0．88％（n=5）。结论联立方程分光光度法简便、快速、可靠,适合于复方苯甲酸醇溶液的快速检测。     

The determination of salicylic acid and benzoic acid in pharmaceutical formulations by spectrofluorimetry.

Methods of extraction from pharmaceutical formulations and subsequent determination of benzoic acid and salicylic acid by spectrofluorimetry are described. The recovery of benzoic acid, in the presence of salicylic acid, was 99.3%, with a coefficient of variation of 1.04%, while the recovery of salicylic acid, in the presence of benzoic acid, was 97.7%, with a coefficient of variation of 0-68%.     

加入合适的稳定剂提高复方水杨酸洗剂的稳定性

目的改善复方水杨酸洗剂的外观质量,提高制剂稳定性。方法以外观色泽为指标,考察单独加入抗氧剂或金属离子络合剂及其联合应用对制剂外观质量的影响。结果合适的稳定剂大幅度延缓了复方水杨酸洗剂的氧化变色速度。加入0.08%以上的硫脲和0.005%的依地酸二钠后基本上抑制了变色现象。结论复方水杨酸洗剂应选择加入合适的稳定剂,解决制剂迅速氧化变质的问题。     

4-氨基水杨酸钠结肠靶向胶囊定位研究

目的：考察4-氨基水杨酸钠结肠定位胶囊体内靶向性。方法：利用X-射线跟踪技术验证4-氨基水杨酸钠口服结肠定位胶囊在人体内的靶向性。结果：4-氨基水杨酸钠结肠定位胶囊在结肠黏附性、靶向性较好。结论：该实验为4-氨基水杨酸钠结肠定位胶囊的研究提供了一定实验基础。