多波长高效液相色谱法同时测定栀子厚朴汤醇提液中6个主要成分的含量

目的:建立同时测定栀子厚朴汤醇提液中栀子苷、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚与厚朴酚含量的高效液相色谱方法。方法:采用Hypersil C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-水为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长为238 nm(0～12 min)、283 nm(12～30 min)、294 nm(30～40 min),柱温30℃。结果:栀子苷、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、厚朴酚的进样量分别在1.03～10.3μg(r=0.9996)、0.184～1.84μg(r=0.9996)、0.880～8.80μg(r=0.9997)、0.478～4.78μg(r=0.9996)、0.221～2.21μg(r=0.9998)、0.538～5.38μg(r=0.9998)范围内与各自峰面积值呈良好线性关系;平均回收率(n=6)分别为99.4%,99.2%,102.4%,100.3%,102.0%,99.8%。结论:本方法简便、准确、可靠,可用于栀子厚朴汤醇提液的质量控制。     

HPLC梯度洗脱法同时测定镇痛活络酊中4种成分的含量

目的建立同时测定镇痛活络酊中香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B含量的高效液相色谱法。方法采用依利特C18柱;流动相为乙腈(A)-0.5%磷酸溶液(B),梯度洗脱;流速:1.3 mL/min;柱温:26℃;检测波长λ_1=254 nm(香蒲新苷及异鼠李素-3-O-新橙皮苷),λ_2=285 nm[巴西苏木素和(±)原苏木素B]。结果香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B的线性范围分别为4.62~92.40μg/mL(r=0.999 2)、5.70~114.00μg/mL(r=0.999 6)、8.95~179.00μg/mL(r=0.999 4)、7.79~155.80μg/mL(r=0.999 7);香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B的平均加样回收率分别为97.81%、99.16%、97.23%、96.74%,其RSD分别为1.19%、0.84%、1.04%、1.08%。结论所建立的镇痛活络酊样品中,4种成分(香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B)的含量测定方法准确、可靠。     

HPLC波长切换法同时测定香砂平胃丸中5种有效成分的含量

目的建立HPLC波长切换法同时测定香砂平胃丸中苍术素、橙皮苷、和厚朴酚、厚朴酚、甘草酸5种有效成分的含量。方法采用Syncronis C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相:乙腈(A)-体积分数为0.05%的磷酸水溶液(B),梯度洗脱,流速:1.0 mL·min~(-1),检测波长:0～18 min时283 nm检测橙皮苷、18～28 min时250 nm检测甘草酸、28～40 min时294 nm检测和厚朴酚与厚朴酚、40～50 min时335 nm检测苍术素,柱温:35℃。结果苍术素、橙皮苷、和厚朴酚、厚朴酚和甘草酸质量浓度分别为5.125～82.00(r=0.999 2,n=6)、19.98～319.6(r=0.999 3,n=6)、12.53～200.4(r=0.999 9,n=6)、15.08～241.2(r=0.999 9,n=6)、15.03～240.4 mg·L~(-1)(r=0.999 9,n=6)时与峰面积呈现良好线性;方法的平均加样回收率为98.4%～99.0%(RSD≤1.7%,n=9)。结论该方法可用于控制和评价香砂平胃丸的质量。     

HPLC法同时测定沉香舒郁丸中四种成分的含量

目的建立波长切换联合梯度洗脱HPLC法同时测定沉香舒郁丸中和厚朴酚、厚朴酚、木香烃内酯和去氢木香内酯4个成分的含量。方法采用Phenomenex C_(18)(250 mm×4.6 mm,5μm),以甲醇(A)-0.5%磷酸溶液(B)为流动相,进行梯度洗脱,流速0.9 mL/min,检测波长:294 nm(和厚朴酚、厚朴酚),225 nm(木香烃内酯、去氢木香内酯),柱温30℃,进样量10μL。结果和厚朴酚、厚朴酚、木香烃内酯和去氢木香内酯4个成分的质量浓度分别在4.30~86.00μg/mL(r=0.999 8)、4.46~89.20μg/mL(r=0.999 5)、5.12~102.40μg/mL(r=0.999 9)、6.18~123.60μg/mL(r=0.999 2)范围内与峰面积呈良好的线性关系;平均加样回收率及相应的RSD分别为98.57%(1.08%)、99.93%(0.73%)、97.26%(1.24%)、97.65%(0.99%);重复性良好,RSD≤1.75%;精密度良好,RSD≤1.06%。供试品溶液在室温条件下24 h内稳定,RSD≤1.11%。平均加样回收率在97.26%~99.93%,RSD≤1.24%。结论所建立的方法专属性好,准确度高,灵敏度高,快速,为沉香舒郁丸的质量控制提供依据。     

HPLC梯度洗脱法同时测定小儿暑感宁糖浆中的香荆芥酚、麝香草酚、和厚朴酚及厚朴酚

目的:建立用高效液相色谱法（HPLC）同时测定小儿暑感宁糖浆中的香荆芥酚、麝香草酚、和厚朴酚及厚朴酚含量的分析方法。方法:采用HPLC法,色谱柱:Eclipse XDB-C₁₈柱（250 mm×4.6 mm,5μm）;流动相为甲醇（A）-0.05%冰醋酸溶液（B）,梯度洗脱;柱温:30℃;流速:1.0 m L·min^-1;进样量:20μL;香荆芥酚、麝香草酚检测波长为λ₁=274 nm,和厚朴酚、厚朴酚检测波长为λ₂=294 nm。结果:香荆芥酚、麝香草酚、和厚朴酚及厚朴酚线性范围分别在6.35¹27.00μg·m L^-1（r=0.999 3）、4.74⁹4.80μg·m L^-1（r=0.999 1）、4.35⁸7.00μg·m L^-1（r=0.999 7）、5.19¹03.80μg·m L^-1（r=0.999 4）范围内线性关系良好。精密度、重现性实验中各组分RSD值均小于2.0%;4种成分的平均加样回收率（n=9）及RSD分别为98.18%（1.15%）、96.94%（1.44%）、99.03%（0.92%）、97.24%（0.79%）。结论:本文建立的HPLC法简便、准确、重复性好,可同时测定小儿暑感宁糖浆中的香荆芥酚、麝香草酚、和厚朴酚及厚朴酚含量,为该制剂的质量控制提供理论参考。     

HPLC法同时测定香砂胃灵散中橙皮苷、和厚朴酚及厚朴酚的含量

目的建立HPLC法同时测定香砂胃灵散中橙皮苷、和厚朴酚及厚朴酚的含量。方法采用HPLC法,色谱柱:Kromasil C_(18)(250 mm×4.6 mm,5μm),流动相:乙腈-水,梯度洗脱,流速:1.0m L·min~(-1),检测波长:290 nm,进样量:20μL,柱温:30℃。结果橙皮苷、和厚朴酚及厚朴酚分别在11.0~110.0(r=0.999 5)、3.6~36.0(r=0.999 7)、5.0~50.0 mg·L~(-1)(r=0.999 4)内与峰面积呈良好的线性关系,平均回收率分别为99.1%、98.9%、98.6%,RSD分别为1.3%、1.1%、1.4%(n=6)。结论该方法可被用于香砂胃灵散的质量控制。     

HPLC法测定胃健宁胶囊中和厚朴酚及厚朴酚的含量

目的建立胃健宁胶囊中和厚朴酚及厚朴酚的检测方法。方法色谱条件为C18色谱柱;流动相:乙腈-水-冰醋酸(60∶40∶1)(V∶V∶V);流速:1.000 mL·min-1;检测波长:294 nm。结果胃健宁胶囊中和厚朴酚在0.02⁰.32μg(r=0.999 6)范围内线性关系良好,平均回收率为96.58%,RSD为1.78%(n=9);厚朴酚在0.019 60.32μg(r=0.999 6)范围内线性关系良好,平均回收率为96.58%,RSD为1.78%(n=9);厚朴酚在0.019 6⁰.313 6μg(r=0.999 8)范围内线性关系良好,厚朴酚的平均回收率为97.29%,RSD为1.39%(n=9)。结论该方法简便,准确度高,可有效控制胃健宁胶囊的质量。     

UPLC法同时测定藿香正气滴丸中7个化学成分

目的建立UPLC法同时测定藿香正气滴丸中欧前胡素、异欧前胡素、橙皮苷、和厚朴酚、厚朴酚、苍术素、甘草酸7个成分的含量。方法采用Waters Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),流动相:乙腈(A)-体积分数为0.2%的甲酸水溶液(B),梯度洗脱,流速:0.4 m L·min-1,柱温:30℃,检测波长:250 nm,检测欧前胡素、异欧前胡素和甘草酸,284 nm检测橙皮苷,290 nm检测和厚朴酚、厚朴酚,336 nm检测苍术素。结果欧前胡素、异欧前胡素、橙皮苷、和厚朴酚、厚朴酚、苍术素、甘草酸质量浓度分别在2.0~80.6、0.6~23.0、15.0~600.0、10.1~403.2、7.5~301.6、1.0~41.6、10.1~202.4 mg·L-1内与峰面积呈良好的线性关系(r≥0.999 5),平均回收率在98.6%~100.9%(RSD≤2.2%,n=9)。结论该方法可用于藿香正气滴丸的质量控制。     

HPLC法测定养胃片中厚朴酚与和厚朴酚

目的:建立养胃片中厚朴酚与和厚朴酚定量分析方法。方法:采用HPLC法,YMC-Pack ODS-A柱(150mm×4.6 mm,5μm)色谱柱;检测波长294 nm;流速1 ml/min;以乙腈-水-冰醋酸(60∶38∶2)为流动相。结果:厚朴酚的线性范围为0.018 828~0.188 28 mg/ml(r=0.999 9);和厚朴酚的线性范围为0.009 792~0.097 92 g/ml(r=0.999 9),回收率分别为100.9%和104.1%(n=6)。结论:本方法准确、专属性强,可作为养胃片的定量分析方法。     

HPLC法同时测定开胸顺气丸中橙皮苷、和厚朴酚与厚朴酚的含量

目的:建立同时测定开胸顺气丸中橙皮苷、和厚朴酚与厚朴酚含量的方法。方法:采用高效液相色谱法。色谱柱为Agi-lentZORBAXSB-C18柱,流动相为甲醇(A)-5%冰醋酸溶液(B)(梯度洗脱),流速为1.0mL·min-1,柱温为40℃,进样量为10μL,检测波长0～20min为284nm、20～65min为294nm。结果:橙皮苷进样量在0.1717～4.292μg范围内(r=0.9998)、和厚朴酚进样量在0.04004～1.001μg范围内(r=0.9994)、厚朴酚进样量在0.09280～4.640μg范围内(r=0.9998)与各自峰面积积分值均呈良好的线性关系;平均回收率分别为99.88%、99.34%、99.34%,RSD分别为0.67%、1.10%、0.86%(n=6)。结论:本法简便、准确、重复性好、精密度高,可更好地控制开胸顺气丸的质量。     

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。     

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.