复方硫酸庆大霉素颗粒含量测定的探讨

目的建立比浊法测定复方硫酸庆大霉素颗粒的含量。方法取新鲜制备金黄色葡萄球菌，临用前以灭菌生理盐水稀释至在580nm波长处透光率约为5％的溶液。培养基中加入量为5％，培养条件为温度37℃，时间3h，培养时分别放置于水浴杯中，取出后在580nm波长处测定。结果复方硫酸庆大霉素颗粒浓度在0．5-1．2u／ml呈良好的线性关系，回收率为99.2％。结论方法简单、快速，且稳定性好。     

双波长光谱法测定复方氯霉素酊中氯霉素与水杨酸的含量

目的：对复方氯霉素酊的含量测定进行研究。方法：采用双波长光谱法不经分离直接测定复方氯霉素酊中氯霉素与水杨酸的含量。选定氯霉素的测定波长为274．5nm,参比波长为326nm;水杨酸的测定波长为290nm,参比波长为260nm。结果：平均回收率：氯霉素为99．4％,RSD为1．8％（n=6),水杨酸为100．1％,RSD为2．1％（n=6)。结论：该方法简便、快速,准确可靠,适用于该制剂的含量测定。     

荧光法测定盐酸特拉唑嗪胶囊的含量

目的 建立荧光法测定盐酸特拉唑嗪胶囊的含量。方法 以甲醇-水-盐酸（300：700：0．9）为溶剂，激发波长为253nm，在发射波长382nm波长处测定荧光强度。结果 在0．009～0．20μg/mL内，线性关系良好（r=0．9997），平均回收率为99．5％，RSD=0．9％。结论 本法操作简便、结果准确，可用于本品的质量控制。     

导数光谱法测定复方苯甲酸醇溶液中两组分含量

目的建立测定复方苯甲酸醇溶液中苯甲酸和水杨酸含量的方法。方法采用二阶导数光谱法在233nm波长处测定苯甲酸的含量，在319nm波长处测定水杨酸含量。结果苯甲酸、水杨酸质量浓度分别在12．16～60．80μg／mL和6．72—33．60μg／mL范围内二阶导数振幅线性关系良好（r=-0．9998和r=-0．99996），平均回收率分别为100．9％和100．5％，RSD分别为1．01％和1．00％（n=5）。结论所用方法简便、快速、准确，可用于复方苯甲酸醇溶液中苯甲酸和水杨酸的含量测定。     

紫外分光光度法测定甲硝唑口颊片的含量

目的：测定甲硝唑口颊片中甲硝唑的含量。方法：采用紫外分光光度法,在277nm波长处测定,空白辅料无干扰。结果：甲硝唑浓度在5～15μg/mL范围内与吸光度有良好的线性关系（r=0．9999）,平均回收率为100．4％,RSD=0,51％。结论：该方法简便、灵敏、准确,可供甲硝唑口颊片的含量测定。     

紫外分光光度法快速测定那格列奈片的含量

目的采用紫外分光光度法快速测定那格列奈片的含量。方法用乙醇作空白，在259nm波长处照分光光度法测定吸收度。结果那格列奈质量浓度在0．1～1．2mg／mL范围内与吸收度线性关系良好，r=0．9997（n=5），平均回收率为99．47％，RSD=1．169％（n=9）。结论紫外分光光度法快捷、简便、灵敏，可作为该产品的快速测定方法。     

吸收系数法测定多潘立酮片的含量、含量均匀度及溶出度

目的：采用吸收系数法测定多潘立酮片的含量、含量均匀度及溶出度。方法：屏除了有机溶媒异丙醇，以0．1mol·L^-1盐酸溶液为溶剂，超声溶解，根据多潘立酮的紫外吸收特征选择284nm为测定波长，利用吸收系数法进行测定。结果：多潘立酮吸收系数E1%1cm为284，RSD0．4％：线性范围6．4～32mg·L^-1（r=0．9998）； 平均回收率（n=9）；100．5％，RSD0．6％。结论：本法简便、实用、环保、准确度高，适用于多潘立酮片含量、含量均匀度及溶出度的测定，可作为多潘立酮片的质量控制方法。     

紫外分光光度法测定布洛芬片含量

目的:建立紫外分光光度法测定布洛芬片的含量。方法:采用氢氧化钠溶液为溶剂,在265nm波长处测定吸收度,绘制标准曲线。结果:该法测定平均回收率为99．97％,RSD为0．17％,线形范围为0．1～0．5mg/ml,r= 0．9995。结论:用本法测定布洛芬片含量简便,快捷,结果与药典法基本一致。     

吸收系数法测定阿司咪唑片的含量、含量均匀度及溶出度

目的：采用吸收系数法测定阿司咪唑片的含量、含量均匀度及溶出度。方法：屏除了有机溶媒异丙醇，以0．1mol·L^-1盐酸溶液为溶剂，超声溶解，根据阿司咪唑的紫外吸收特征选择277nm为测定波长，利用吸收系数法进行测定。结果：阿司咪唑吸收系数E1cm^1%为296，RSD=0．7％；线性范围4～20nag·L^-1（r=0．9997）；平均回收率（n=9）：100．3％，RSD=0．5％。结论：本法简便、实用、环保、准确度高，适用于阿司咪唑片含量、均匀度及溶出度的测定，可作为阿司咪唑片的质量控制方法。     

碘酸钾口服液含量测定波长的选择

目的探讨碘酸钾口服液含量测定波长的选择。方法在530nm和580nm波长处用紫外分光光度法对不同包装的样品进行了质量对比。结果两个波长含量测定结果基本一致,但塑料瓶装样品留样考察两年半后含量下降近50％。结论考虑到KIO,最大吸收波长580nm已作为国家药典中该品种的含量测定波长,建议将碘酸钾口服液的含量检测波长由530nm改为580nm;产品包装选择棕色玻璃瓶。     

乙酰螺旋霉素片的工艺研究

目的：筛选乙酰螺旋霉素片最佳处方。方法：考察预胶化淀粉、低取代羟丙基纤维素和吐温－８０对乙酰螺旋霉素片的质量影响,并与２种市售乙酰螺旋霉素片作溶出度比较。结果：筛选的最佳处方制备的乙酰螺旋霉素片,体外溶出度大为提高。结论：本法处方合理,工艺简单,适用于工业化生产。     

Studies on acetylspiramycin. 1. Separation and chemical structures of acetylspiramycin components

1. A macrolide antibiotic acetylspiramycin (ASPM) was separated into seven fractions using high performance liquid chromatography (HPLC) with Lichrosorb RP-8 and mobile phase of a mixed solvent of 0.025M phosphate ammonium (pH 7.4) and acetonitrile at a ratio of 10:18. 2. Five components were purified over 90%, and analyzed using mass spectroscopy, 1H NMR, and 13C NMR, and their chemical structures were determined as 4'-acetylspiramycin I, 4'-acetylspiramycin II, 4'-acetylspiramycin III, 3',4'-diacetylspiramycin II and 3',4'-diacetylspiramycin III, respectively. 3. The weight component ratio of the seven fractions of ASPM separated by HPLC was constant throughout several lots of ASPM which had been stocked for nearly 15 years at room temperature, indicating an excellent chemical stability of the antibiotic. 4. Some physicochemical parameters were determined for the five ASPM components. Solubilities in water at 24 degrees C were in a range from 0.14 mg/ml to 4.9 mg/ml, and they were, in the decreasing order, 3',4'-diacetylspiramycin III, 3',4'-diacetylspiramycin I 4'-acetylspiramycin III, 4'-acetylspiramycin II, and 4'-acetylspiramycin I. Relationships between solubilities and numbers and positions of acyl substituents in spiramycin molecule are discussed.     

比浊法自动测定乙酰螺旋霉素片的效价

目的 建立比浊法测定乙酰螺旋霉素片的方法.方法 金葡菌为实验菌,加菌量约0.5%(V/V),(37士0.5)℃培养3.5～4.5h测定.结果 抗生素线性浓度为3.2～15.6μg/ml,平均回收率为100.7%(n=9),RSD=1.4%.结论 本方法操作方便、快速,灵敏、可信限率低,结果准确,精密度好,可作为乙酰螺旋霉素片效价的测定方法.     

乙酰螺旋霉素片剂和胶囊剂的抗菌作用比较

目的比较乙酰螺旋霉素片剂和胶囊剂的体外抗菌作用。方法将乙酰螺旋霉素随机分为片剂组和胶囊组,2组均进行药物体外抗菌实验,测定其对大肠杆菌、金黄色葡萄球菌、枯草芽孢杆菌及绿脓杆菌的最小抑菌浓度（MIC）和最小杀菌浓度（MBC）,对2组的抗菌作用进行比较。结果片剂组MIC及MBC值均高于胶囊组,差异均有统计学意义（P〈0.05）。结论乙酰螺旋霉素片剂抗菌效果优于胶囊剂,可将片剂作为抗菌作用的最佳剂型。     

Experience in treatment of Mycoplasma pneumoniae with acetylspiramycin

Antibiotics of tetracycline and macrolide groups are mainly used in treatment of Mycoplasma pneumonia. In this study, acetylspiramycin (ASPM), an antibiotic of macrolide group, was given to 15 cases of Mycoplasma pneumoniae who visited this institute during the period from January, 1980 to March, 1981, and its clinical effects and side effects were investigated. The therapeutic effects were evaluated by days to the normal body temperature, to improvement in cough and to improvement in X-ray findings. The increase in serum antibody value was adopted as the diagnostic index of Mycoplasma infection. The patients who entered into this study were 7 males and 8 females, ranged from 19 to 60 years of age with an average of 36.3 years. The daily dose of ASPM was 600 to 1,200 mg (potency), and the mean administration period was 18.1 days. The results obtained were as follows. 1. The temperature fell to the normal within 2 to 7 days. 2. Cough disappeared in 2 days at shortest and in 55 days at longest. The mean period of cough disappearance was 14.5 days. 3. In 10 cases who could be followed up, shadows in X-ray films disappeared in 3 days at shortest and in 40 days at longest. The mean period to shadow disappearance was 18.6 days. 4. As regards clinical effects, marked improvement was obtained in 2 cases, improvement in 9, slight improvement in 4, and no change in 0 (improvement rate: 73.3%). 5. As a side effect, nausea was found in 1 case, but it was improved by discontinuance of administration.     

克拉霉素和乙酰螺旋霉素对铜绿假单胞菌生物被膜的作用

目的 :研究克拉霉素 (CAM)、乙酰螺旋霉素 (ASM)对铜绿假单胞菌生物被膜 (BF)合成的影响及其与环丙沙星 (CIP)的相互作用。方法 :色氨酸法测定BF中的多糖蛋白复合物 (GLX) ;高氯酸 蒽酮反应物法定量测定BF的己糖成分 ;噻唑兰法测定活菌数。结果 :1/ 16最低抑菌浓度 (MIC)、1/ 4MIC的CAM可抑制BF中GLX、己糖的合成 ,且可显著增强 1/ 4MIC、1/ 2MIC的CIP对有BF的铜绿假单胞菌的杀菌作用 (P <0 0 5 ) ,而ASM则无以上作用。结论 :CAM可抑制铜绿假单胞菌BF的形成 ,并可增强CIP对有BF的铜绿假单胞菌的杀菌作用 ;而ASM则无抑制铜绿假单胞菌BF的作用     

乙酰螺旋霉素对黄芩苷血药浓度的影响

目的:研究口服乙酰螺旋霉素对黄芩有效成分黄芩苷血药浓度的影响。方法:用HPLC-ECD方法测定乙酰螺旋霉素(333 mg·kg-1,ig,bid,3 d)和黄芩苷(34 mg·kg-1,ig,一次给药)合并给药组与黄芩苷(34 mg·kg-1, ig,一次给药)单独给药组大鼠的血浆黄芩苷浓度,比较二者的药动学参数。结果:乙酰螺旋霉素和黄芩苷合并给药组大鼠黄芩苷血浆浓度的Cmax=(785．84±401．23)ng·mL-1,AUC0-24h=(11 564．27±5 585．65)ng·h·mL-1;黄芩苷单独给药组大鼠黄芩苷血浆浓度的Cmax=(2 645．62±601．42)ng·mL-1,AUC0-24h=(28 952．90±5 731．42) ng·h·mL-1,两组药动学参数存在显著性差异(P<0．05)。结论:口服乙酰螺旋霉素严重影响黄芩苷的血药浓度,提醒临床医生和患者应合理用药。     

乙酰螺旋霉素片微生物限度检查方法验证

目的建立乙酰螺旋霉素片微生物限度检查方法。方法采用常规法、离心沉淀集菌+薄膜过滤法进行方法验证。结果乙酰螺旋霉素片细菌计数采用离心沉淀集菌+薄膜过滤法,霉菌及酵母菌计数采用常规法,控制菌采用离心沉淀集菌+薄膜过滤法。结论确立了乙酰螺旋霉素片微生物限度检查方法 ,保证微生物限度检查方法的有效性。     

乙酰螺旋霉素的液/液界面电化学研究

目的：研究乙酰螺旋霉素的液／液界面转移电化学特性。方法：利用循环伏安法记录乙酰螺旋霉素在水／硝基苯界面转移的循环伏安曲线,计算转移过程的热力学常数。结果：乙酰螺旋霉素在pH2-9范围通过水／硝基苯界面转移,标准转移电位为162mv,标准转移自由能为－1．5KJ/mol。结论：乙酰螺旋霉素的液／液界面转移过程为扩散控制的可逆过程。研究结果有助于对乙酰螺旋霉素的药理和药效的深入认识。     

Studies on acetylspiramycin. II. Biological activities of spiramycin components

Acetylspiramycin (ASPM) was fractionated using high performance liquid chromatography (HPLC). The peak fractions were named F1 to F7 successively in order of increasing retention times (Rt), i.e., increasing hydrophobicity, and studied for 1) antibacterial activities (MIC), 2) antibacterial potency against Bacillus subtilis ATCC 6633, 3) therapeutic effect on mice infected with Streptococcus pneumoniae III, Staphylococcus aureus Smith, 4) acute toxicity by i.p. administration to mice (LD50) and 5) cytotoxicities to fibroblasts derived from Chinese-hamster lung (CHL), cow pulmonary artery endothelial cells (CPAE) and rat hepatic cells. The results obtained are summarized below. 1. Components F1 and 4'-acetylspiramycin F2 had significantly different biological activities from those of other components: F1 showed the lowest antibacterial potency of 492 micrograms (potency)/mg, F2 showed the highest antibacterial potency of 2,040 micrograms (potency)/mg and correspondingly the lowest LD50 value of 692 mg/kg (the highest toxicity). The therapeutic effect of F2 on infections in mice was found to be the second smallest and was superior only to that of F1. The LD50 value of F1 was 1,200 mg/kg and similar to that of ASPM. 2. Antibacterial potencies of F3, F4, F5 and F6 were 1,165, 1,266, 1,374 and 1,530 micrograms (potency)/mg, respectively; fraction with the higher antibacterial activities corresponded to the longer retention times, i.e., the greater hydrophobicities. The most hydrophobic component, F7, 3-propionyl-3",4"-diacetylspiramycin, however, showed a low antibacterial potency of 1,085 micrograms (potency)/mg, next to the lowest one, F1, a fact which was in contradiction to with the sequential relation between hydrophobicities and potencies from F3 to F6.(ABSTRACT TRUNCATED AT 250 WORDS)