HPLC法同时测定六味能消丸中8种成分的含量

目的:建立同时测定六味能消丸中土木香内酯、异土木香内酯、没食子酸、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚含量的方法。方法:采用高效液相色谱法。色谱柱为Diamonsil C_(18),流动相为甲醇-乙腈-0.1%冰醋酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm(土木香内酯、异土木香内酯、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚)、270 nm(没食子酸),柱温为25℃,进样量为10μL。结果:土木香内酯、异土木香内酯、没食子酸、芦荟大黄素、大黄酸、大黄素、大黄素甲醚、大黄酚检测进样量线性范围分别为0.121～3.63μg(r=0.999 9)、0.122～3.66μg(r=0.999 9)、0.219～6.57μg(r=0.999 9)、0.016 4～0.492μg(r=0.999 7)、0.017 3～0.519μg(r=0.999 9)、0.015 3～0.459μg(r=0.999 9)、0.007 2～0.216μg(r=0.999 9)、0.016 2～0.486μg(r=0.999 9);定量限分别为0.41、0.26、0.35、0.13、0.17、0.14、0.15、0.13 ng,检测限分别为0.12、0.08、0.11、0.04、0.05、0.04、0.05、0.04 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为98.05%～102.46%(RSD=1.75%,n=6)、98.55%～102.89%(RSD=1.91%,n=6)、98.53%～102.34%(RSD=1.66%,n=6)、101.71%～103.41%(RSD=0.57%,n=6)、101.04%～103.01%(RSD=0.69%,n=6)、101.63%～102.75%(RSD=0.39%,n=6)、96.94%～101.11%(RSD=1.61%,n=6)、98.06%～99.10%(RSD=0.40%,n=6)。结论:该方法准确、简便,可用于六味能消丸中8种成分含量的同时测定。     

用HPLC法同时测定六味安消胶囊中土木香内酯、异土木香内酯、大黄素和大黄酚的含量

目的：建立HPLC法同时测定六昧安消胶囊中土木香内酯、异土木香内酯、大黄素和大黄酚含量的方法。方法：采用HPLC-二极管阵列检测器法（HPLC—DAD），色谱柱：Agilent Eclipse PlusC18柱（250mm×4.6mm，5μm），流动相：乙腈-0．04％甲酸（60：40），流速：1．0mL／min，检测波长：220nm，柱温：25℃，进样量：10μL。结果：土木香内酯、异土木香内酯、大黄素和大黄酚的线性范围分别是：2．46～98．4、2．48～99．2、2．56～102．4和2．58～103．2μg／mL，色谱响应线性关系良好。日内和日间RSD均〈2％；最低检测限分别为1．75、1．31、0．50和0．49μg／mL。稳定性结果为峰面积的RSD分别为1．29％、1．40％、1．30％和0．45％，在48h内稳定。加样回收率结果分别为99．0％、100．6％、98．7％和99．7％（n＝6），RSD分别为1．03％、0．62％、1．36％和0．26％。结论：本法快速、简便，重现性好，精密度高，测定结果准确可靠，可作为该制剂的定量测定方法。     

HPLC法同时测定六味能消胶囊中木香烃内酯、去氢木香烃内酯大黄素、大黄酚的含量

目的:建立六味能消胶囊中木香烃内酯、去氢木香烃内酯、大黄素、大黄酚4个成分含量测定的方法。方法:采用Atlantis C18色谱柱(150 mm×4.6 mm,5μm),以甲醇-0.1%磷酸水为流动相,梯度洗脱,检测波长225 nm(0~25 min检测木香烃内酯、去氢木香烃内酯)、254 nm(25~40 min检测大黄素、大黄酚),柱温25℃。结果:木香烃内酯、去氢木香烃内酯、大黄素、大黄酚的线性范围分别为0.665 6~33.28、0.563 7~31.84、0.524 8~26.24、0.585 6~29.28μg·m L-1;平均回收率(n=6)分别为99.28%(RSD=1.8%),101.7%(RSD=1.6%),101.2%(RSD=2.0%),99.36%(RSD=1.8%)。5批样品中木香烃内酯、去氢木香烃内酯、大黄素、大黄酚含量分别为2.32~2.41、2.48~2.62、0.42~0.48、1.26~1.33 mg·g-1。结论:该方法可用于六味能消胶囊中木香烃内酯、去氢木香烃内酯、大黄素、大黄酚的同时测定。     

HPLC法同时测定利胆解毒胶囊中异土木香内酯和土木香内酯的含量

目的:建立高效液相色谱法(HPLC)同时测定利胆解毒胶囊中异土木香内酯和土木香内酯含量的方法.方法:采用Diamonsil Plus C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.05％磷酸溶液(50:50),流速1.0 mL·min-1,检测波长210 nm,柱温30.0℃.结果:异土木香内酯...     

果旭阿汤中土木香内酯和异土木香内酯的含量测定

［摘要］目的建立同时测定藏药果旭阿汤中土木香内酯和异土木香内酯含量的方法。方法通过优化提取方法,用气相色谱（GC）法同时测定藏药果旭阿汤中藏木香有效成分土木香内酯和异土木香内酯的含量。结果土木香内酯和异土木香内酯均在0.1～1.0 mg&#8226;mL-1 (n=5）范围内呈良好线性关系。土木香内酯回收率为97.25% (n=6),RSD=0.93%;异土木香内酯回收率为97.42% (n=6), RSD=0.90%。结论该方法可用于藏药果旭阿汤中土木香内酯和异土木香内酯的含量同时快速、准确测定。     

HPLC法测定大黄通便颗粒中大黄素和大黄酚的含量

建立大黄通便颗粒中大黄素和大黄酚含量的HPLC测定方法.采用Spherixorb C18色谱柱,流动相:甲醇-0.1%磷酸溶液(90:10),流速:0.8ml·min-1,检测波长:254nm.线性范围:大黄素0.0135～0.2160μg(r=0.9998),大黄酚0.0240～0.3840μg(r=0.9995).平均加样回收率(n=5)分别为大黄素100.8%,RSD=1.1%;大黄酚100.2%,RSD=0.8%.本法简便,快速,结果准确.     

高效液相色谱法测定中药退黄外洗液中大黄酸、大黄素、大黄酚的含量

目的 建立中药退黄外洗液中大黄酸、大黄素、大黄酚的含量测定方法.方法 采用高效液相色谱(HPLC)法测定大黄酸、大黄素、大黄酚的含量,色谱柱:Phenomenex Gemini 5μm C18 110A 4.6×250.0mm 5micron;流动相:甲醇-0.1%磷酸溶液(85:15),流速:1.0ml/min,检测波长:254nm,柱温:35℃.结果 大黄酸在1.6576～33.1520μg/ml、大黄素在1.4976～29.9520μg/ml、大黄酚在1.7040～34.0800μg/ml范围内线性关系良好(r=1).大黄酸平均回收率为99.07%,RSD为0.85%(n=5);大黄素为99.14%,RSD为1.08%(n=5);大黄酚为99.94%,RSD为0.77%(n=5);阴性对照无干扰.结论 该方法操作简便、稳定、专属性强,可作为该制剂的质量控制方法.     

高效液相色谱法测定中药退黄外洗液中大黄酸、大黄素、大黄酚的含量

目的建立中药退黄外洗液中大黄酸、大黄素、大黄酚的含量测定方法。方法采用高效液相色谱(HPLC)法测定大黄酸、大黄素、大黄酚的含量,色谱柱:Phenomenex Gemini5μm C18110A4.6×250.0mm5micron;流动相:甲醇-0.1%磷酸溶液(85∶15),流速:1.0ml/min,检测波长:254nm,柱温:35℃。结果大黄酸在1.6576～33.1520μg/ml、大黄素在1.4976～29.9520μg/ml、大黄酚在1.7040～34.0800μg/ml范围内线性关系良好(r=1)。大黄酸平均回收率为99.07%,RSD为0.85%(n=5);大黄素为99.14%,RSD为1.08%(n=5);大黄酚为99.94%,RSD为0.77%(n=5);阴性对照无干扰。结论该方法操作简便、稳定、专属性强,可作为该制剂的质量控制方法。     

高效液相色谱法测定沉香曲中羌活醇、异欧前胡素、木香烃内酯和去氢木香内酯的含量

目的建立HPLC法测定沉香曲中羌活醇、异欧前胡素、木香烃内酯和去氢木香内酯的含量。方法色谱柱为Hypersil C18柱(4.6 mm×250 mm,5μm);流速:0.9 mL·min-1;检测羌活醇和异欧前胡素的流动相为乙腈-0.5%磷酸溶液(67:33),检测波长:312 nm;检测木香烃内酯和去氢木香内酯的流动相为乙腈-甲醇-1%冰醋酸溶液(45:24:31),检测波长:225 nm。结果羌活醇和异欧前胡素进样量分别在0.018 6⁰.372 0μg(r=0.999 2)、0.011 20.372 0μg(r=0.999 2)、0.011 2⁰.224 0μg(r=0.999 1)与峰面积呈良好的线性关系,平均加样回收率分别为96.6%、98.0%,RSD分别为1.6%、1.2%(n=6);木香烃内酯和去氢木香内酯进样量分别在0.041 40.224 0μg(r=0.999 1)与峰面积呈良好的线性关系,平均加样回收率分别为96.6%、98.0%,RSD分别为1.6%、1.2%(n=6);木香烃内酯和去氢木香内酯进样量分别在0.041 4⁰.828 0μg(r=0.999 5)、0.010 80.828 0μg(r=0.999 5)、0.010 8⁰.216 0μg(r=0.999 7)与峰面积呈良好的线性关系,平均加样回收率分别为98.0%、96.2%,RSD分别为1.4%、1.1%(n=6)。结论该方法测定结果准确性强、灵敏度高、重复性好。     

HPLC-DAD法同时测定七珍汤散（努布炖屯汤）中4个成分

目的:建立HPLC-DAD法同时测定七珍汤散中没食子酸、6-姜辣素、异土木香内酯、土木香内酯的含量,为七珍汤散的质量控制研究、考察其处方各味藏药材的成分和质量标准的提高提供参考。方法:采用Luna C₁₈色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.2%醋酸溶液,梯度洗脱(0～10min,2%→12%A;10～20 min,12%→50%A;20～30 min,50%→85%A;30～50 min,85%→2%A),流速1.0 mL·min^-1,柱温35℃,检测波长230、280 nm。结果:4种成分实现完全分离;没食子酸、6-姜辣素、异土木香内酯、土木香内酯的线性范围依次分别在7.42～148.4、0.92～18.4、1.83～91.25、1.71～85.30μg(r≥0.9990);平均加样回收率依次分别为99.06%、99.27%、99.86%、99.36%,RSD依次分别为1.33%、0.67%、0.35%、0.18%。结论:该方法对4个成分同时测定,简便准确,重复性好,灵敏度高,阴性试验无干扰,可用于七珍汤散的质量控...     

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.