RP-HPLC法同时测定辣椒碱透皮贴剂中4种生物碱类成分的含量

目的建立RP-HPLC法同时测定辣椒碱透皮贴剂中辣椒碱、二氢辣椒碱、降二氢辣椒碱和高二氢辣椒碱4种生物碱类成分含量。方法采用Kromasil C_(18)(250 mm×4.60 mm,5μm)柱,以乙腈-水(体积比为42∶58)为流动相,流速为1.0 mL·min~(-1),柱温为40℃,检测波长为280 nm。结果 4种生物碱类成分的色谱峰与邻近色谱峰均能良好的分离,辣椒碱和二氢辣椒碱的质量浓度分别在2.65～79.50 mg·L~(-1)(r=0.999 7)、1.08～64.80 mg·L~(-1)(r=0.999 9)内与峰面积呈良好的线性关系,平均回收率分别为100.2%(RSD=1.5%)、99.5%(RSD=0.7%)。结论该方法可用于辣椒碱透皮贴剂的质量控制。     

HPLC法测定辣椒总碱中辣椒碱及二氢辣椒碱的含量

在 C6H5键合硅胶为填充剂的色谱柱上 ,以乙腈 - 0 .1% H3 PO4(33∶ 6 7)为流动相 ,检测波长为 2 80 nm,同时测定了辣椒总碱中辣椒碱及二氢辣椒碱的含量。结果表明 ,辣椒总碱中辣椒碱及二氢辣椒碱的含量约为5 8%和 30 % ,方法的平均加样回收率分别为 98.2 %和 97.6 %。     

RP-HPLC法测定辣椒中辣椒素、二氢辣椒素和降二氢辣椒素含量

目的:建立反相高效液相色谱法同时测定辣椒中辣椒素、二氢辣椒素和降二氢辣椒素含量。方法:采用Nucleosil C18(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-水,梯度洗脱,流速1.0 mL.min-1,检测波长280 nm,柱温45℃,外标法定量。结果:3个辣椒碱的线性关系良好,线性范围均为1.0～160.0μg.mL-1,相关系数在0.9991～0.9995之间;精密度、稳定性试验的RSD均低于3%;辣椒素、二氢辣椒素和降二氢辣椒素平均回收率(n=6)分别为96.4%,98.1%,99.3%,RSD分别为2.6%,2.1%,1.2%;检出限分别为0.2,0.1,0.1μg.mL-1。结论:该方法简便快捷,应用本方法测定了10个品种辣椒中3个辣椒碱的含量,结果稳定。     

RP-HPLC法测定辣椒中辣椒碱的含量

目的:建立以反相高效液相色谱法测定辣椒中辣椒碱含量的方法。方法:色谱柱为Zorbax Eclipse XDB-C18(150mm×4.6mm,5μm),流动相为乙腈-0.1%磷酸溶液(45∶55,pH2.6),流速为1.0mL·min-1,柱温为40℃,检测波长为281nm。结果:辣椒碱检测浓度在30～70mg·L-1范围内与峰面积积分值呈良好线性关系(r=0.9999);平均加样回收率为101.33%,RSD=1.57%(n=9)。结论:本方法操作简便、快速,结果准确,可用于辣椒中辣椒碱的含量测定。     

HPLC法测定仲景胃灵丸中8种成分及其化学计量学综合评价

目的建立HPLC梯度洗脱法同时测定仲景胃灵丸中茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氢紫堇碱、紫堇碱和四氢小檗碱,并采用化学计量学方法对其结果进行分析评价。方法采用HPLC法,Agilent Zorbax SB C_(18)色谱柱(250 mm×4.6 mm,5μm),柱温30℃;乙腈–0.1%冰醋酸水溶液为流动相,梯度洗脱,体积流量0.9 mL/min;进样量10μL;检测波长分别为248 nm(检测茴香醛)、280 nm(检测肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氢紫堇碱、紫堇碱和四氢小檗碱)。采用统计软件对仲景胃灵丸中8种成分的质量分数进行化学计量学评价。结果茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氢紫堇碱、紫堇碱、四氢小檗碱分别在0.96～24.00、1.78～44.50、20.06～501.50、3.92～98.00、2.89～72.25、2.13～53.25、1.36～34.00、0.59～14.75μg/mL线性关系良好;平均加样回收率分别为96.97%、97.81%、100.04%、99.13%、98.91%、96.89%、97.58%、98.34%,RSD值分别为1.04%、1.51%、0.54%、1.01%、0.92%、1.32%、1.36%、1.41%。化学计量学表明10批仲景胃灵丸聚为3类,主成分1～4是影响仲景胃灵丸整体质量的主要因子。结论以茴香醛、肉桂醇、肉桂酸、桂皮醛、延胡索乙素、去氢紫堇碱、紫堇碱、四氢小檗碱同步测定的HPLC法和化学计量学方法可用于仲景胃灵丸多指标质量评价。     

HPLC测定复方苦参凝胶剂中苦参碱与辣椒碱的含量

目的:应用高效液相色谱法测定复方苦参凝胶剂中辣椒碱与苦参碱的含量.方法:采用WatersμBONDAPAK C18柱(3.9 mm×300mm,5 μm),乙腈-0.05 mol·L-1磷酸二氢钠溶液-三乙胺(50:50:0.05);用磷酸调整pH值至2.2为流动相;检测波长为227 nm;流速:1.0 ml·min-.结果:辣椒碱线性范围为6.25～200μg·ml-1(r=0.999 9,n=5);苦参碱线性范围为80.0～800.0 μg·ml-1(r=0.999 7,n=5).辣椒碱平均回收率为101.8%(n=9),RSD=1.8%;苦参碱平均回收率为100.7%(n=9),RSD=0.9%.结论:本方法用于凝胶剂中辣椒碱与苦参碱含量的测定简便、快速、灵敏、结果准确.     

反相高效液相色谱法测定辣椒风湿软膏中总辣椒碱含量

目的用反相高效液相色谱法（RP—HPLC法）测定辣椒风湿软膏中总辣椒碱的含量。方法采用ZorbaxC18柱（250mm×4．6mm，5pm）；流动相为甲醇-2．5％乙酸溶液（60：40），流速为2．0mL／min，检测波长为280nm，进样量为20μL。结果方法的线性范围为2-200μg／mL（r=1．0000），精密度RSD为0．45％（n=5），加样回收率为98．64％（RSD为0．72％）。结论RP～HPLC法具有专属、灵敏、快速、准确等优点，可用于辣椒风湿软膏中总辣椒碱含量的测定。     

HPLC法同时测定双黄消炎片中黄芩苷、药根碱、巴马汀及小檗碱的含量

目的:用 HPLC 法同时测定双黄消炎片中黄芩苷和3种生物碱类成分药根碱、巴马汀及小檗碱的含量。方法:色谱柱:Diamonsil~(TM)(钻石)C_(18)柱(250 mm×4.6 mm,5μm);流动相:0.1%磷酸(加三乙胺调 pH 至2.97)-乙腈(75:25);流速:1.0 mL·min~(-1);检测波长:345 nm。结果:黄芩苷、药根碱、巴马汀和小檗碱分别在0.13～2.7μg(r=0.9998),0.0097～0.19μg(r=0.9998),0.010～0.20μg(r=0.9999),0.020～0.40μg(r=0.9998)范围内线性关系良好;4个成分的平均回收率(n=9)分别为100.4%,99.7%,100.1%,100.4%。结论:本方法快速、简便,重复性好,可作为该制剂的质量控制方法。     

高效液相色谱法测定小儿腹泻凝胶膏中吴茱萸碱及吴茱萸次碱含量

目的建立测定小儿腹泻凝胶膏中吴茱萸碱及吴茱萸次碱含量的高效液相色谱(HPLC)法。方法小儿腹泻凝胶膏中加入80%乙醇超声提取吴茱萸碱及吴茱萸次碱,采用HPLC法,色谱柱为Cosmosil 5 C18-MS-Ⅱ柱(250 mm×4.6 mm,5μm),乙腈-水(51∶49)为流动相,流速为1.0 mL/min,检测波长为225 nm,进样量为10μL。结果吴茱萸碱和吴茱萸次碱进样量分别在0.089～0.89μg和0.077～0.768μg范围内与峰面积呈良好线性关系,吴茱萸碱和吴茱萸次碱的平均回收率为97.80%和99.87%,RSD为0.88%和1.27%。结论该方法简单、准确、重现性好,可用于小儿腹泻凝胶膏中吴茱萸碱及吴茱萸次碱的含量测定。     

复方辣椒碱乳膏的药物释放性能研究

目的研究复方辣椒碱乳膏的药物释放性能。方法采用液质联用法检测复方辣椒碱乳膏中辣椒碱的体外释放性能。液相色谱柱为zorbaxXDBc—s柱（150mm×2．1mm,3．5μm）,流动相为甲醇一水（80：20）,质谱检测仪离子源为Esi源;采用气相色谱法同时检测复方辣椒碱乳膏中水杨酸甲酯、薄荷脑和樟脑的体外释放性能,气相色谱柱为DB一624毛细管柱（30m×0．53mm,3．0μm）,FID检测器,分流进样,分流比为5：1,进样口温度220℃,检测器温度250℃,柱温100℃保持3rain,以5℃／min升至200℃,保持5min。结果根据所含活性成分的溶解度确定了释放介质,建立了液质联用与气相色谱测定方法,测定了各成分的释放。结论液质联用法可用于研究复方辣椒碱乳膏中微量辣椒碱的的释放行为,能够准确检测辣椒碱的体外释放性能;气相色谱法可用于研究水杨酸甲酯、薄荷脑和樟脑的释放行为,能够准确检测水杨酸甲酯、薄荷脑和樟脑的释放性能。     

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。     

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。     

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.     

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.