高效液相色谱法同时测定西替利嗪/麻黄素滴鼻剂中二组分的含量

目的用HPLC法同时测定滴鼻剂中盐酸西替利嗪和盐酸麻黄素的含量.方法采用C18色谱柱(4.6mm × 150mm,5μm),流动相为甲醇-0.01mol·L-1磷酸二氢钠(60:40),检测波长230nm和257nm(0～3min:257nm;3～15min:230nm).结果盐酸西替利嗪和盐酸麻黄素在40～400μg·mL-1浓度内呈良好线性关系,平均回收率分别为99.56%和101.12%,RSD分别为%1.13和1.02%(n=3).结论该方法可同时测定滴鼻剂中盐酸西替利嗪和盐酸麻黄素的含量.     

高效液相色谱法测定山丹酮缓释片中牡荆苷和金丝桃苷的含量

建立高效液相色谱法测定山丹酮缓释片中牡荆苷和金丝桃苷的含量.色谱柱Lichrospher C18(5μm, 250mm×4.6mm), 流动相:甲醇-水-冰醋酸(50∶50∶1);检测波长:340 nm;牡荆苷和金丝桃苷的线性范围分别为:0.73～3.66μg(r=0.9999)和0.63～3.16μg (r=0.9998);平均回收率分别为:100.03%,RSD=1.17% (n=5)和99.81%,RSD=0.36%(n=5).本法操作简单,快速,准确,可行.     

非那西丁及其代谢产物对乙酰氨基酚的高效液相色谱测定

目的建立非那西丁及其代谢产物对乙酰氨基酚的高效液相色谱测定方法.方法色谱柱:Nova-PakR C18(3.9 mm×150 mm,5μm);流动相为甲醇水溶液,其梯度洗脱程序为:17%(体积分数,下同)甲醇(保持5 min)→80%甲醇(10 min)→17%甲醇(12 min);检测波长254 nm.结果非那西丁、对乙酰氨基酚线性范围分别为0.687～87.920 μg/mL(r=0.9999,n=5),0.423～54.200μg/mL(r=0.9997,n=5).低、中、高三种浓度的平均方法回收率非那西丁为96.9%(n=5),对乙酰氨基酚为95.1%(n=5); 日内,日间精密度(RSD)均小于6%(n=5).结论本研究为非那西丁的药物代谢研究提供了一种测定方法.     

HPLC测定蕨菜中的槲皮素和山萘酚

目的 采用HPLC法测定蕨菜中的槲皮素和山萘酚.方法 采用Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-0.04%磷酸(48:52),流速1.0 ml·min-1,检测波长360 nm,柱温35℃.结果 两种成分均达到基线分离,槲皮素和山萘酚的线性范围分别为0.029～0.200 μg和0.0034～0.0119 μg;r分别为0.9999和0.9998;平均回收率分别为102.7%(RSD=2.0%,n=6)和98.5%(RSD=1.7%,n=6).结论 所建方法快速、准确,可作为蕨菜药材质量控制的有效方法.     

HPLC法同时测定黄芩中黄芩苷、黄芩素、汉黄芩素的含量

目的:建立反相高效液相色谱法同时测定黄芩中黄芩苷、黄芩素、汉黄芩素的含量.方法:采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-0.1％磷酸溶液为流动相,梯度洗脱;检测波长为277 nm;流速1.0 ml·min -1;进样量10 μl;柱温35℃.结果:黄芩苷、黄芩素、汉黄芩素的线性范围分别为0.059 ～ 1.175 μg,r=1.000 0(n =7)、0.010～0.204μg,r=1.000 0(n =7)和8.210×10-3～1.642×10-1 μg,r =1.000 0(n =7);提取回收率分别为99.08％,RSD=0.5％(n=6)、98.66％,RSD =0.5％ (n =6)和98.31％,RSD =0.7％ (n =6).结论:本法操作简便、快速、结果准确,可用于黄芩的质量控制.     

高效液相色谱法测定白癜精药散中补骨脂素和异补骨脂素的含量

目的:建立白癜精药散的补骨脂素和异补骨脂素的含量测定方法.方法:高效液相色谱法,色谱柱为Agilent Zoxbox C18柱(5μm,4.5 mm×250mm);流动相为甲醇-水(47:53);检测波长为245 nm;柱温为35℃;流速为1.0 mL/min.结果:补骨脂素线性范围是0.216～1.08μg,回归方程为Y=1.264×10-7X-7.713×10-4,r=0.999 9(n=5);异补骨脂素线性范围是0.228～1.14μg,回归方程为Y=1.313×10-7X-3.008×10-4,r=0.999 8(n=5).补骨脂素与异补骨脂素的平均回收率分别为99.2%与99.1%,RSD分别为1.93%和1.87%(n=5).结论:高效液相色谱法简便、快速、灵敏、准确,重现性好.     

HPLC法同时测定消炎片中绿原酸、秦皮乙素和咖啡酸的含量

目的:建立HPLC法同时测定消炎片中绿原酸、秦皮乙素和咖啡酸的含量.方法:采用Agilent Eclipse XDB-C18 (250mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-0.04％磷酸溶液为流动相,梯度洗脱;检测波长为328 nm;流速1.0ml·min -1;进样量20μl;柱温35℃.结果:绿原酸、秦皮乙素和咖啡酸的线性范围分别为1.616 ～40.400μg·ml-1(r=0.999 9,n=7)、5.164～129.100μg ·ml-1(r=1.000 0,n=7)和1.344～ 26.880 μg·ml-1(r=1.000 0,n=7);提取回收率分别为99.08％(RSD=0.6％,n=6)、98.81％(RSD =0.4％,n=6)和98.92％(RSD=0.9％,n=6).结论:本法操作简便、快速、结果准确.     

毛细管气相色谱和HPLC法检测头孢美唑中的残留溶剂

目的 建立测定头孢美唑原料药中残留溶剂甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚、N,N-二甲基苯胺的检测方法.方法 用Agilent HP-5毛细管气相色谱柱和氢焰离子化检测器,按顶空进样的方式同时测定了头孢美唑中甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚的残留量.用高效液相色谱法,以甲醇-水(75:25)为流动相,检测波长254nm,测定头孢美唑中N,N-二甲基苯胺.结果 甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚、N,N-二甲基苯胺的线性范围分别为121.5～607.5μg/mL(r=0.9997,n=5)、199.8～998.9μg/mL(r=0.9998,n=5)、199.5～1247.1μg/mL(r=0.9999,n=5)、15.6～125.2μg/mL(r=0.9993,n=6)、249.5～1247.7μg/mL(r=0.9993,n=5),0.096～0.256μg/mL(r=0.9995,,n=5);3种浓度的平均加样回收率(n=3)为91.34%～104.84%(RSD为1.2%～6.5%).结论 两种检测方法简单,可靠,可以用于头孢美唑原料药的质量控制.     

HPLC测定芍甘胶囊中的甘草酸和甘草苷

目的 建立HPLC测定芍甘胶囊中甘草酸和甘草苷含量的方法.方法 色谱柱为Kromasil C18(250 mm×4.6 mm,5 μm).甘草酸单铵盐以甲醇-0.2 mol·l-1醋酸铵溶液-冰醋酸(65:35:1)为流动相,检测波长250 nm,流速1.0 ml·min-1;甘草苷以乙腈-0.5%冰醋酸(18:82)为流动相,检测波长276 am,流速1.0 ml·min-1.结果 甘草酸单铵盐和甘草苷的线性范围分别为0.52～2.60、0.30～1.50μg(r=0.9998);平均回收率分别为98.1%(RSD=1.32%,n=5)、97.0%(RSD=1.67%,n=5).结论 所建方法灵敏、准确、专属性强,可作为芍甘胶囊的质量控制方法.     

HPLC法测定天麻素氯化钠注射液中天麻素的含量

目的:建立HPLC定天麻素氟化钠注射液中天麻素的含量.方法:用Hypersil BDS(5μm,4.6mm*250mm)C18柱;以甲醇-0.01mol/L磷酸二氢钠(8:92,磷酸调节pH至4.0±0.1)为流动相;流速0.8ml/min;检测波长220nm;进样量20μl.结果:天麻素在2.5μg/ml～25μg/ml范围内,天麻素浓度与峰面积的线性关系良好(r=0.9998),检测限为1.15ng(S/N=3).回收率为98.9%,RSD=0.08%(n=9).结论:方法简便,结果准确,重复性好.     

Safety assessment of poloxamers 101, 105, 108, 122, 123, 124, 181, 182, 183, 184, 185, 188, 212, 215, 217, 231, 234, 235, 237, 238, 282, 284, 288, 331, 333, 334, 335, 338, 401, 402, 403, and 407, poloxamer 105 benzoate, and poloxamer 182 dibenzoate as used in cosmetics

Poloxamers are polyoxyethlyene, polyoxypropylene block polymers. The impurities of commercial grade Poloxamer 188, as an example, include low-molecular-weight substances (aldehydes and both formic and acetic acids), as well as 1,4-dioxane and residual ethylene oxide and propylene oxide. Most Poloxamers function in cosmetics as surfactants, emulsifying agents, cleansing agents, and/or solubilizing agents, and are used in 141 cosmetic products at concentrations from 0.005% to 20%. Poloxamers injected intravenously in animals are rapidly excreted in the urine, with some accumulation in lung, liver, brain, and kidney tissue. In humans, the plasma concentration of Poloxamer 188 (given intravenously) reached a maximum at 1 h, then reached a steady state. Poloxamers generally were ineffective in wound healing, but were effective in reducing postsurgical adhesions in several test systems. Poloxamers can cause hypercholesterolemia and hypertriglyceridemia in animals, but overall, they are relatively nontoxic to animals, with LD(50) values reported from 5 to 34.6 g/kg. Short-term intravenous doses up to 4 g/kg of Poloxamer 108 produced no change in body weights, but did result in diffuse hepatocellular vacuolization, renal tubular dilation in kidneys, and dose-dependent vacuolization of epithelial cells in the proximal convoluted tubules. A short-term inhalation toxicity study of Poloxamer 101 at 97 mg/m(3) identified slight alveolitis after 2 weeks of exposure, which subsided in the 2-week postexposure observation period. A short-term dermal toxicity study of Poloxamer 184 in rabbits at doses up to 1000 mg/kg produced slight erythema and slight intradermal inflammatory response on histological examination, but no dose-dependent body weight, hematology, blood chemistry, or organ weight changes. A 6-month feeding study in rats and dogs of Poloxamer 188 at exposures up to 5% in the diet produced no adverse effects. Likewise, Poloxamer 331 (tested up to 0.5 g/kg day(-1)), Poloxamer 235 (tested up to 1.0 g/kg day(-1)), and Poloxamer 338 (at 0.2 or 1.0 g/kg day(-1)) produced no adverse effects in dogs. Poloxamer 338 (at 5.0 g/kg day(-1)) produced slight transient diarrhea in dogs. Poloxamer 188 at levels up to 7.5% in diet given to rats in a 2-year feeding study produced diarrhea at 5% and 7.5% levels, a small decrease in growth at the 7.5% level, but no change in survival. Doses up to 0.5 mg/kg day(-1) for 2 years using rats produced yellow discoloration of the serum, high serum alkaline phosphatase activity, and elevated serum glutamicpyruvic transaminase and glutamic-oxalacetic transaminase activities. Poloxamers are minimal ocular irritants, but are not dermal irritants or sensitizers in animals. Data on reproductive and developmental toxicity of Poloxamers were not found. An Ames test did not identify any mutagenic activity of Poloxamer 407, with or without metabolic activation. Several studies have suggested anticarcinogenic effects of Poloxamers. Poloxamers appear to increase the sensitivity to anticancer drugs of multidrug-resistant cancer cells. In clinical testing, Poloxamer 188 increased the hydration of feces when used in combination with a bulk laxative treatment. Compared to controls, one study of angioplasty patients receiving Poloxamer 188 found a reduced myocardial infarct size and a reduced incidence of reinfarction, with no evidence of toxicity, but two other studies found no effect. Poloxamer 188 given to patients suffering from sickle cell disease had decreased pain and decreased hospitilization, compared to controls. Clinical tests of dermal irritation and sensitization were uniformly negative. The Cosmetic Ingredient Review (CIR) Expert Panel stressed that the cosmetic industry should continue to use the necessary purification procedures to keep the levels below established limits for ethylene oxide, propylene oxide, and 1,4-dioxane. The Panel did note the absence of reproductive and developmental toxicity data, but, based on molecular weight and solubility, there should be little skin penetration and any penetration of the skin should be slow. Also, the available data demonstrate that Poloxamers that are introduced into the body via routes other than dermal exposure have a rapid clearance from the body, suggesting that there would be no risk of reproductive and/or developmental toxicity. Overall, the available data do not suggest any concern about carcinogenesis. Although there are gaps in knowledge about product use, the overall information available on the types of products in which these ingredients are used, and at what concentration, indicates a pattern of use. Based on these safety test data and the information that the manufacturing process can be controlled to limit unwanted impurities, the Panel concluded that these Poloxamers are safe as used.     

HPLC法测定抗妇炎胶囊中木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱

目的 采用高效液相色谱（HPLC）法同时测定抗妇炎胶囊中木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱10种活性成分。方法 采用InerSustain AQ-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,流动相A：乙腈–无水乙醇（80∶20）,流动相B：0.1%磷酸溶液,梯度洗脱,检测波长220 nm,体积流量1.0 mL/min,柱温30℃,进样量10 μL。结果 木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱分别在2.69～134.50、1.95～97.50、0.63～31.50、0.86～43.00、11.95～597.50、0.59～29.50、6.08～304.00、4.85～242.50、1.66～83.00、19.79～989.50 μg/mL线性关系良好（r≥0.999 3）;平均回收率分别为99.11%、98.23%、96.95%、97.78%、100.02%、97.21%、99.66%、99.52%、98.81%、100.08%,RSD值分别为1.04%、1.23%、1.37%、1.65%、0.70%、1.28%、0.65%、0.81%、1.11%、0.63%。结论 建立的HPLC法可用于抗妇炎胶囊中10种活性成分的测定,作为抗妇炎胶囊质量控制方法。     

Arformoterol: (R,R)-eformoterol, (R,R)-formoterol, arformoterol tartrate, eformoterol-sepracor, formoterol-sepracor, R,R-eformoterol, R,R-formoterol

Sepracor in the US is developing arformoterol [R,R-formoterol], a single isomer form of the beta(2)-adrenoceptor agonist formoterol [eformoterol]. This isomer contains two chiral centres and is being developed as an inhaled preparation for the treatment of respiratory disorders. Sepracor believes that arformoterol has the potential to be a once-daily therapy with a rapid onset of action and a duration of effect exceeding 12 hours. In 1995, Sepracor acquired New England Pharmaceuticals, a manufacturer of metered-dose and dry powder inhalers, for the purpose of preparing formulations of levosalbutamol and arformoterol. Phase II dose-ranging clinical studies of arformoterol as a longer-acting, complementary bronchodilator were completed successfully in the fourth quarter of 2000. Phase III trials of arformoterol began in September 2001. The indications for the drug appeared to be asthma and chronic obstructive pulmonary disease (COPD). However, an update of the pharmaceutical product information on the Sepracor website in September 2003 listed COPD maintenance therapy as the only indication for arformoterol. In October 2002, Sepracor stated that two pivotal phase III studies were ongoing in 1600 patients. Sepracor estimates that its NDA submission for arformoterol, which is projected for the first half of 2004, will include approximately 3000 adult subjects. Sepracor stated in July 2003 that it had completed more than 100 preclinical studies and initiated or completed 15 clinical studies for arformoterol inhalation solution for the treatment of bronchospasm in patients with COPD. In addition, Sepracor stated that the two pivotal phase III studies in 1600 patients were still progressing. In 1995, European patents were granted to Sepracor for the use of arformoterol in the treatment of asthma, and the US patent application was pending.     

欧洲刺柏（Juniper）

活性成分与药理作用欧洲刺柏药用部位是其浆果，具有促水排泄、防腐、抗胃肠胀气和抗风湿作用，还可改善胃功能。用作促水排泄药可增加尿量（水丢失），但不增加钠排泄。成分萜品烯-4-醇可增加肾小球滤过率，但刺激肾。欧洲刺柏浆果对单纯疱疹病毒体外显示抗病毒活性，并具抗真菌活性。动物实验显示，欧洲刺柏浆果提取物具有堕胎、抗生育、抗炎、抗胚胎植入、降血压、升血压和降血糖作用。欧洲刺柏浆果油具有兴奋子宫的活性，以及利尿、胃肠道抗菌和刺激作用，该油对平滑肌有阻止解痉作用。     

Oral Presentations (LDD, LPES, LNM, LPAT, LNT, LPPT, LPM)

Probiotic microorganisms have been shown to provide specific health benefits when consumed as food supplements or as food components. The main problem of such products is the poor survival of the probiotic bacteria in the low pH of gastric fluid. However the use of synthetic excipients for enteric coating to prevent the exposure of microorganisms to gastric fluid is limited in food supplementary industry. Therefore the aim of this study was to develop an enteric coating formulation containing shellac as a natural polymer. Shellac possesses good resistance to gastric juice; the major disadvantage of this polymer is its low solubility in the intestinal fluid [1, 2]. Thus films containing different ratios of shellac and water-soluble polymers (sodium alginate, hydroxypropyl methylcellulose (HPMC) and polyvinylpyrrolidon (PVP)) or plasticizers (glycerol and glyceryl triacetate (GTA)) were prepared in order to analyse the films’ melting temperatures (T_m), the changes in enthalpy (ΔH), their capability of taking up water, and their solubility in different media. The release characteristics of the films were studied by loading pellets with Enterococcus faecium M74 and coating them with formulations containing different amounts of shellac and polymer or plasticized shellac. Using dissolution tests, performed according to USP XXXI paddle method, the resistance of the coatings to simulated gastric fluid (SGF, pH 1.2) and the release of cells in simulated intestinal fluid (SIF, pH 6.8) was investigated.The trials showed that an increasing amount of plasticizer results in a decrease of T_m and ΔH of the films whereat glycerol had a superior plasticization effect to GTA. The compatibility of films made of water-soluble polymers and shellac was also concentration dependent. HPMC and PVP showed superior compatibility with shellac compared to sodium alginate, since films containing shellac and more than 10% [w/w] sodium alginate tended to separate into two phases. In the end five formulations containing shellac and either 5% [w/w] glycerol, 10% [w/w] PVP, 20% [w/w] PVP, 10% [w/w] HPMC, or 5% [w/w] sodium alginate emerged as feasible for enteric coating purposes.