高效液相色谱法同时测定麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量

目的建立麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量测定方法。方法采用奥泰ALLTIMA-C18色谱柱(4.6 mm×250 mm,5μm),以甲醇(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱[0~9min,60%A;9~20 min,60%→80%A;20~45 min,80%A];流速:1.0 mL.min-1;柱温:30℃;检测波长254 nm。结果大黄素、大黄酸、大黄酚、大黄素甲醚、芦荟大黄素线性范围分别为在9.08~81.72、8.4~75.6、13.42~120.7、7.56~68.04、8.2~73.8μg.mL-1,与峰面积线性关系良好,平均回收率分别为99.1%、99.6%、99.4%、99.8%、99.2%,RSD分别为2.0%、1.8、3.2%、1.1%、1.5%。结论本方法可作为麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素含量测定的一种准确、灵敏、可行的方法。     

HPLC法测定夏黄颗粒中芦荟大黄素、大黄酸、厚朴酚、和厚朴酚、大黄素、大黄酚和大黄素甲醚

目的建立HPLC法同时测定夏黄颗粒中芦荟大黄素、大黄酸、厚朴酚、和厚朴酚、大黄素、大黄酚和大黄素甲醚。方法采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm);流动相:甲醇–0.1%磷酸水溶液,梯度洗脱;检测波长254 nm;体积流量1.0 m L/min;柱温30℃;进样体积20μL。结果芦荟大黄素、大黄酸、厚朴酚、和厚朴酚、大黄素、大黄酚、大黄素甲醚分别在23.8~238.4、22.8~228.0、25.8~228.0、78.7~787.2、16.7~167.2、16.6~166.4、17.5~175.2μg线性关系良好;平均加样回收率分别为99.78%、99.36%、99.71%、98.65%、99.37%、99.42%、98.78%,RSD值分别为1.88%、2.05%、2.03%、2.01%、2.56%、2.35%、2.17%。结论本法快速、简便、准确,可用于夏黄颗粒的质量控制。     

HPLC法测定枳实导滞丸中芦荟大黄素、大黄酸、大黄素、大黄酚及大黄素甲醚的含量

目的:建立枳实导滞丸中芦荟大黄素、大黄酸、大黄素、大黄酚及大黄素甲醚的含量测定方法。方法:采用HPLC法,色谱柱:Waters Symmery C₁₈（250mm×4.6mm,5μm）,流动相:甲醇-0.1%磷酸水溶液（85:15）,检测波长:254nm,流速:1.0ml·ml^-1。结果:芦荟大黄素、大黄酸、大黄素、大黄酚及大黄素甲醚的线性范围分别为0.011～0.226μg（r=0.9998）、0.005～0.092μg（r=0.9999）、0.010～0.194μg（r=0.999 9）、0.011～0.212μg（r=0.9999）、0.005～0.102μg（r=0.9998）;浓度范围内进样量与峰面积线性关系良好。平均回收率分别为97.47%（RSD=1.56%）、99.57%（RSD=0.91%）、100.66%（RSD=1.09%）、101.97%（RSD=1.60%）、101.54%（RSD=1.58%）（n=6）。结论:所建方法简单、快速、准确,可用于枳实导滞丸的质量控制。     

HPLC法测定胆石通胶囊中芦荟大黄素、大黄酸、大黄素、大黄酚及大黄素甲醚的含量

目的建立同时测定胆石通胶囊中芦荟大黄素、大黄酸、大黄素、大黄酚及大黄素甲醚的含量测定方法。方法以UltimateTM XB-C18(250 mm×4.6 mm,5μm)为色谱柱,柱温:35℃;流动相:甲醇-1 g·L-1磷酸溶液,梯度洗脱;流速:1.0 mL·min-1;检测波长:430 nm;进样量10μL。结果芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚分别在60.02~1 200.4,70.32~1 406.4,62.24~1 244.8,71.04~1 420.8和30.48~609.6 ng范围内呈良好线性关系,相关系数分别为0.999 9,0.999 9,0.999 9,0.999 5和0.999 9,平均回收率分别为98.1%,99.3%,98.4%,99.0%和99.2%。结论该方法专属性好,准确度高,可用于综合评价胆石通胶囊的质量。     

HPLC法测定通腑胶囊中大黄素、大黄酸、大黄酚、大黄素甲醚及芦荟大黄素的含量

目的建立高效液相色谱法测定通腑胶囊中大黄素、大黄酸、大黄酚、大黄素甲醚及芦荟大黄素含量的方法。方法采用HPLC法,色谱柱:Waters C18(250×4.6mm,5μm),以0.1%磷酸:甲醇(15∶85)为流动相,流速1.0μL/min,检测波长:254nm,柱温:35℃。结果大黄素、大黄酸、大黄酚、大黄素甲醚及芦荟大黄素进样量分别在0.0162~0.323μg、0.016~0.318μg、0.0164~0.328μg、0.008~0.16μg、0.020~0.406μg范围内进样量与峰面积积分值呈良好的线性关系,相关系数均为0.9999,平均回收率分别为:99.0%、99.0%、99.2%、98.3%、99.4%(n=6)。结论该方法专属性强,重现性好,可用于通腑胶囊中蒽醌类成分的含量测定。     

HPLC法测定金花消痤丸中大黄酸、大黄素、大黄酚及大黄素甲醚的含量

目的建立金花消痤丸中大黄酸、大黄素、大黄酚、大黄素甲醚的含量测定法。方法采用HPLC法测定含量:Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,0.1%磷酸—甲醇(24∶76)为流动相,检测波长254 nm,流速1.0 mL·min-1;柱温:30℃。结果大黄酸、大黄素、大黄酚、大黄素甲醚分离完全,平均加样回收率分别为96.6%、95.7%、97.4%、95.1%。结论该方法简便,快速,准确。     

HPLC法测定导赤丸中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量

目的制定测定导赤丸中芦荟大黄酸、大黄素、大黄酚、大黄素和大黄素甲醚5种活性成分含量的方法。方法利用高效液相色谱法进行测定,采用流动相A:100%乙腈-0.1%磷酸,B:10%乙腈-0.1%磷酸以梯度浓度洗脱;流速控制在1mL/min;波长设定为254nm;柱温30℃。结果芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚质量浓度与峰面积均呈良好的线性关系,平均回收率分别为99.7%(RSD为1.28%n=5),99.1%(RSD为1.68%n=5),99.6%(RSD为0.90%n=5),98.8%(RSD为0.89%n=5),99.7%(RSD为1.04%n=5)。结论本法结果准确,操作简便,可靠,重复性好,可用于导赤丸的质量控制。     

HPLC法测定柔肝降脂胶囊中橙黄决明素、芦荟大黄素、大黄酚和大黄素甲醚

目的 建立柔肝降脂胶囊中橙黄决明素、芦荟大黄素、大黄酚和大黄素甲醚的HPLC测定方法。方法 采用Waters Symmetry C₁₈色谱柱（250 mm×4.6 mm,5 μm）;流动相为甲醇–0.1%磷酸水溶液,梯度洗脱;检测波长288 nm;体积流量为1.0 mL/min;柱温30℃;进样量10 μL。结果 橙黄决明素、芦荟大黄素、大黄酚、大黄素甲醚的线性范围分别为1.59～51.00、0.87～27.92、1.63～52.17、0.22～7.06 μg/mL。平均回收率分别为97.55%、100.40%、98.75%、101.30%,RSD值分别为1.93%、1.53%、1.77%、2.23%。4种蒽醌类成分中橙黄决明素和大黄酚的质量分数较高,大黄素甲醚的质量分数较低,不同批次柔肝降脂胶囊样品中芦荟大黄素的质量分数差异较明显。结论 所建立的方法可用于柔肝降脂胶囊中4种蒽醌类成分的测定,可为柔肝降脂胶囊的质量控制研究提供参考。     

用HPLC法测定牛黄上清片中各大黄素成分的含量

目的:建立HPLC同时测定牛黄上清片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚含量的方法.方法:色谱柱为Shimadzu VP-ODS柱(4.6 mm×250 mm,5 mm),流动相为乙腈-0.1%磷酸梯度洗脱,流速为1.0 ml/min,检测波长为254 nm,柱温30℃.结果:芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在0.042～0.840μg(r=0.9996)、0.168～3.352μg(r=0.9998)、0.084～1.680 μg(r=0.9997)、0.093～1.852μg(r=0.9999)和0.174～3.488μg(r=0.9994)内呈良好线性关系,平均回收率分别为99.8%(RSD=1.34%)、99.8%(RSD=1.72%)、100.0%(RSD=0.89%)、99.5%(RSD=0.97%)和100.2%(RSD=1.04%).结论:本方法简便、快速、准确,可用于牛黄上清片的质量控制.     

高效液相色谱法同时测定九制大黄丸中5组分含量

目的 建立同时测定九制大黄丸中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量的高效液相色谱(HPLC)法。方法 色谱柱为C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(77∶23),流速1.0 m L/min,检测波长254 nm,柱温40℃,进样量20μL。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的进样质量浓度线性范围分别为4.6~92μg/m L,3.8~76μg/m L,4.0~800μg/m L,5.0~100μg/m L和17.6~352μg/m L,平均回收率分别为99.38%,99.04%,99.72%,99.59%和99.52%,RSD分别为0.80%,1.02%,0.50%,0.54%,0.92%(n=6)。结论 HPLC法可同时测定九制大黄丸中5组分的含量,专属性强,分离效果好。     

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.