气相色谱法测定亚微乳凝胶剂中樟脑、薄荷脑、水杨酸甲酯的含量

目的:建立气相色谱法测定亚微乳凝胶剂中樟脑、薄荷脑、水杨酸甲酯含量的方法。方法:气相色谱柱为 SE-54柱(30m×0.32 mm,0.25μm);环己酮为内标。采用 FID 检测器,进样口温度230℃,检测器温度250℃,采用程序升温,起始温度90℃,保持5 min,以10℃·min~(-1)升到150℃,保持2 min。结果:樟脑、薄荷脑、水杨酸甲酯线性范围分别为0.18～1.60 mg·mL~(-1)(r=0.9999),0.17～1.55 mg·mL~(-1)(r=0.9998),0.40～3.59 mg·mL~(-1)(r=0.9999);平均回收率分别为99.5%,99.2%,99.1%;RSD 均小于2%(n=9)。结论:本法方便,准确,重现性好,可作为本制剂的质量控制方法。     

气相色谱法测定止痒消炎水中薄荷脑、冰片和麝香草酚的含量

目的建立同时测定止痒消炎水中薄荷脑、冰片和麝香草酚含量的气相色谱测定方法。方法采用气相色谱内标法,FID检测器,HP-INNDW AX石英毛细管柱(30m×250μm,0.25μm),应用程序升温(140℃保持4.1min以后20℃.min-1升至240℃),进样口温度200℃,检测器温度250℃;分流进样,分流比10:1。结果薄荷脑在0.32～3.2mg.mL-1,冰片在0.56～5.6mg.mL-1,麝香草酚在0.16～1.6mg.mL-1内呈良好的线性关系,加样回收率,薄荷脑为99.8%,(RSD=1.3%);冰片为99.2%(RSD=1.5%);麝香草酚为99.8%(RSD=0.9%)。结论该方法简单可靠,适合于止痒消炎水中薄荷脑、冰片和麝香草酚的含量测定。     

气相色谱法同时测定拜尼多中4种有效成分含量

目的:建立气相色谱法同时测定拜尼多(康松无极膏)中薄荷脑、樟脑、水杨酸甲酯及麝香草酚的含量。方法:采用气相色谱法,色谱柱为INNOWAX石英毛细管柱(0.32 mm×30 m,0.25μm),采用程序升温法,检测器温度为250℃。结果:薄荷脑、樟脑、水杨酸甲酯及麝香草酚的回归方程分别为Y=190375.67 9507.62X(r=0.9999),Y=80436.70 9030.67X(r=0.9995),Y=73630.95 6474.46X(r=0.9999),Y=8653.41 432.18X(r=0.9998);线性范围分别为108.2—1406.6,422.0—2100.0,100.7—906.3,8.3—75.5μg·mL~(-1);回收率分别为102.6%-105.5%,109.5%-119.0%,104.0%-107.5%,100.6%-104.3%。结论:该法快速、准确、可靠,适用于康松无极膏的含量测定。     

高效液相色谱法同时测定复方樟脑乳膏中樟脑和水杨酸甲酯的含量

目的建立高效液相色谱(HPLC)法同时测定复方樟脑乳膏中樟脑和水杨酸甲酯含量的方法,并与气相色谱(GC)法比较。方法 HPLC法采用Alltima C18(150 mm×4.6 mm,5μm)色谱柱,紫外检测器,乙腈-10%甲醇水(50∶50)为流动相,流速为0.8 mL·min~(-1),樟脑和水杨酸甲酯的检测波长分别为287 nm和304 nm。GC法采用Rtx-wax色谱柱(30 m×0.25 mm,0.25μm),FID检测器,柱温为120℃,保持20 min,萘为内标。结果 HPLC法中樟脑和水杨酸甲酯分别在0.202～2.0175mg·mL~(-1)和0.025 24～0.8076 mg·mL~(-1)与相对应色谱峰峰面积线性关系良好;GC法中樟脑和水杨酸甲酯分别在0.5038～3.779 mg·mL~(-1)和0.3929～2.947 mg·m L-1与其峰面积与内标峰面积的比值线性关系良好。水杨酸甲酯和樟脑的平均回收率分别为98.7%～99.3%,99.1%～99.5%(HPLC法);100.1%～100.7%,99.4%～100.6%(GC法);RSD值均<2.0%(n=3)。样品测定结果进行统计分析,差异无统计学意义。结论 HPLC法与GC法均可以用于复方樟脑乳膏中樟脑和水杨酸甲酯的含量测定,GC法略优于HPLC法,但HPLC法更适合医疗机构中含樟脑和水杨酸甲酯成分制剂的质量控制。     

GC法测定香薷感冒滴丸中麝香草酚和香荆芥酚的含量

目的:建立气相色谱法测定香薷感冒滴丸中麝香草酚和香荆芥酚的含量。方法:色谱柱为 HP-17石英毛细管柱(HP50%PhMe Silicone,10m×0.25mm×0.25μm),柱初始温度130℃,停留14min,以20℃·min~(-1)速度一阶升温至220℃,停留36min。结果:麝香草酚在12.5～125.1μg·mL~(-1)(r=0.9998),香荆芥酚在21.5～215.2μg·mL~(-1)(r=0.9997)范围内有良好的线性关系;平均回收率分别为麝香草酚101.4%(RSD=2.7%),香荆芥酚98.7%(RSD=2.3%),重复性的 RSD 分别为麝香草酚2.3%,香荆芥酚2.0%。结论:本方法可靠、准确,专属性强,可以作为控制香薷感冒滴丸质量的方法。     

复方水杨酸甲酯苯海拉明喷雾剂中5个活性成分的含量测定

目的:建立气相色谱法同时测定复方水杨酸甲酯苯海拉明喷雾剂中水杨酸甲酯、薄荷脑、樟脑、麝香草酚和盐酸苯海拉明的含量。方法:采用聚乙二醇20M毛细管色谱柱(30 m×0.53 mm, 1.0μm),氦气为载气,氢火焰离子检测器,程序升温(起始温度为160℃,维持10 min,再以50℃·min^-1的速率,升温至230℃,维持12 min),进样口温度200℃;检测器温度250℃,萘为内标。结果:水杨酸甲酯、薄荷脑、樟脑、麝香草酚和盐酸苯海拉明的质量浓度分别在1.504～4.512、1.198～3.594、1.910～5.730、0.148 4～0.445 2、0.091 07～0.273 2 mg·mL^-1范围内与各相应成分峰和内标峰的峰面积比值呈良好线性关系(r均>0.999,n均为5);低、中、高3个浓度水平9份样品的平均加样回收率分别为99.0%(RSD=0.65%)、99.9%(RSD=0.62%)、101.6%(RSD=0.73%)、102.5%(RSD=1.1%)、100.1%(RSD=1.8%);精密度、稳定性良好,RSD均&...     

气相色谱法测定止痒消炎水中冰片、薄荷脑和麝香草酚的含量

目的建立气相色谱法测定止痒消炎水中的冰片、薄荷脑和麝香草酚的含量。方法采用聚乙二醇毛细管柱(30m×0.25mm×0.25μm),FID检测器,程序升温:初始温度110℃,7℃/min升至200℃,分流进样,分流比为20∶1。结果3种成分的线性关系良好,平均回收率(n=6)分别为薄荷脑100.7%,RSD为1.2%;冰片100.4%,RSD为1.2%;麝香草酚100.8%,RSD为1.4%。结论方法简便、快速、准确。     

GC外标法测定伤湿止痛膏中挥发性成分的含量

目的 建立了毛细管GC法测定伤湿止痛膏中樟脑、薄荷脑、冰片、水杨酸甲酯的含量测定.方法 采用DB-WAX毛细管柱,FID检测器,挥发油提取法净化样品,乙酸乙酯为稀释溶剂.结果 樟脑平均回收率96.8%;RSD为1.1%、薄荷脑平均回收率97.3%;RSD为1.4%、冰片平均回收率96.4%;RSD为0.9%;水杨酸甲酯平均回收率97.0%;RSD为1.1%.结论 改方法 简单、准确、重复性好,为伤湿止痛膏的质量控制提高提供了依据.     

气相色谱法测定活血消痛酊中樟脑、薄荷脑、龙脑和异龙脑的含量

目的建立气相色谱(GC)法同时测定活血消痛酊中樟脑、薄荷脑、龙脑和异龙脑的含量。方法采用Agilent DB-WAX毛细管色谱柱(30 m×0.32 mm,0.25μm);FID检测器;进样口温度:230℃;检测器温度:250℃;柱温:程序升温,起始温度60℃,保持2 min,以15℃·min~(-1)升至160℃,保持4 min。结果樟脑、薄荷脑、龙脑和异龙脑的线性范围分别为0.054～2.720(r_1=1.000 0),0.018～0.890(r_2=0.999 9),0.017～0.870(r_3=1.000 0)和0.021～1.050 mg·mL~(-1)(r_4=1.000 0);平均回收率(n=6)分别为98.5%,99.5%,97.4%和96.4%;RSD值分别为0.6%,0.6%,0.7%和0.7%。结论该方法简便、可靠,重复性好,可用于活血消痛酊的质量控制。     

GC同时测定消炎镇痛膏中的樟脑、薄荷脑、龙脑和水杨酸甲酯

目的 建立同时测定消炎镇痛膏中樟脑、薄荷脑、龙脑和水杨酸甲酯含量的方法.方法 采用GC法,以萘为内标物,色谱柱为HP-INNOMAX毛细管柱(30 m×0.32 mm,1.0 μm),进样口温度为200℃,FID检测器温度为250℃;采用程序升温,起始温度为140℃,保持17 min,以50℃·min-1的速率升至180℃,保持5 min.结果 樟脑、薄荷脑、龙脑和水杨酸甲酯的线性范围分别为0.062～6.200 μg(r=0.9999)、0.097～9.700 μg(r:0.9998)、0.045～4.500 μg(r=0.9999)、0.045～4.500μg(r=0.9999),平均加样回收率分别为95.2%、96.8%、95.7%和96.4%,RSD均小于3%(n=9).结论 所建方法快速、简便、准确,可有效地控制消炎镇痛膏的质量.     

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.