HPLC-CAD法测定浓维磷糖浆中果糖、葡萄糖、蔗糖和麦芽糖含量

目的 建立高效液相色谱串联电喷雾检测器（HPLC - CAD）同时测定浓维磷糖浆中果糖、葡萄 糖、蔗糖和麦芽糖含量的方法,为其质量标准提高提供依据。方法 采用Alltech chrom Prevail carbohydrate ES 5u色谱柱(4.6 mm×250 mm,5 μm),以乙腈-水（75∶25）为流动相,流速 1.0 mL·min^-1,柱温 35 ℃。电喷雾检测器参数为：雾化温度35 ℃,采样频率10 Hz。结果 上述4个糖类成分分离完全,线性关系良好（r均大于0.999 0）;精密度、重复性及回收率实验结果均符合含量测定要求,果糖、葡萄糖、蔗糖和麦芽糖的平均加样回收率分别为98.4%、97.5%、99.4%和95.4%。结论 该方法灵敏度高、准确可靠,可用于于浓维磷糖浆中果糖、葡萄糖、蔗糖和麦芽糖含量测定。     

UPLC-MS/ELSD法快速检测板蓝根颗粒及组分中的糖类成分

目的 建立板蓝根颗粒及组分中糖类成分的快速定性方法和主要单糖的定量测定方法。方法 采用超高效液相色谱结合质谱检测器（UPLC-MS）快速定性板蓝根颗粒及组分中的糖类成分,采用超高效液相色谱结合蒸发光散射检测器（UPLC-ELSD）同时测定果糖、葡萄糖的含量。使用ACQUITY UPLC BEH Amide（2.1 mm×150 mm,1.7 μm）色谱柱分离,柱温35℃。流动相分别为乙腈-0.1%氨水（含10 mmol/L碳酸氢铵）（75：25）和乙腈（含0.2%三乙胺）-水（75： 25）,体积流量0.2 mL/min。质谱检测器采用负离子模式,毛细管电压0.8 V,锥孔电压4 V,探头温度600℃,采集频率1 Hz,采用全扫描及SIR扫描模式。ELSD检测器漂移管温度50℃,氮气压力275.8 kPa。结果 经UPLC-MS法鉴定板蓝根颗粒中糖类成分种类为单糖和双糖,主要为果糖、葡萄糖、蔗糖、肌醇,水洗脱组分检出果糖、葡萄糖、蔗糖,10%醇洗脱组分和20%醇洗脱组分均检出蔗糖。UPLC-ELSD法含量测定结果表明,果糖、葡萄糖在各自范围内线性关系良好,各相关系数均0.999 3在以上,平均回收率分别为99.0%、100.1%。28个生产企业的28批样品糖类成分含量差异较大。结论 所建立的方法准确度、重复性良好,具有操作简便、节省时间等特点,可为板蓝根颗粒的质量控制和物质基础研究提供参考。     

HPLC-CAD法同时测定蜂蜜中的果糖、葡萄糖、蔗糖和麦芽糖含量

摘 要 目的：建立高效液相色谱 电喷雾检测器（HPLC CAD）同时测定蜂蜜中果糖、葡萄糖、蔗糖和麦芽糖含量的方法。方法: 使用Alltech Prevail carbohydrate ES（250 mm×4.6 mm,5 μm）色谱柱,流动相为乙腈 水(70〖KG*9〗∶〖KG-*2〗30),流速为0.8 ml·min^-1,柱温为30℃,采用电喷雾检测器进行检测。结果: 各分析物分离完全,线性关系良好,各相关系数均在0.999 8以上,加样回收率在96.94%～99.23%,检测限为0.93～1.85 mg·L^-1。结论: 所建立的方法灵敏度高,准确性、重复性良好,具有操作简单、节省时间、环保等特点,可用于蜂蜜中果糖、葡萄糖、蔗糖和麦芽糖的质量控制。     

HPLC-ELSD同时测定丹参川芎嗪注射液中间体中7种糖类成分

目的 建立同时测定丹参川芎嗪注射液中间体中果糖、葡萄糖、蔗糖、蜜二糖、棉子糖、甘露三糖和水苏糖7种糖类成分的HPLC-ELSD方法，并研究丹参川芎嗪注射液生产过程中糖类成分的变化规律。方法 采用Prevail Carbohydrate ES色谱柱（250 mm×4.6 mm，5 μm），以乙腈-水为流动相进行梯度洗脱，柱温为25 ℃，进样量为5 μL，流速为0.6 mL·min^–1，ELSD检测器雾化器温度为70 ℃，漂移管温度为60 ℃，氮气流量1.0 L·min^–1。结果 7种糖类成分在定量范围内线性关系良好，R²均>0.998 0，进样、日内、日间和中间精密度RSD值均<5%，供试品溶液在10 h内稳定，低、中、高浓度平均加样回收率为97.00%~104.34%。结论 建立的分析方法稳定、准确、重复性好，可用于丹参川芎嗪注射液中间体中7种糖类成分含量测定。本研究推进了丹参川芎嗪注射液安全性再评价质量控制研究，也为其他中药制剂中糖类成分的定量、转移、转化规律研究提供了参考。     

基于HPLC-CAD的参麦颗粒中糖含量与色度值的相关性分析及糖摄入量评估

目的 建立高效液相色谱串联电喷雾检测器（HPLC-CAD）同时测定参麦颗粒中三种糖类成分含量的方法，结合色度值分析参麦颗粒色泽与糖类含量的相关性，为参麦颗粒处方制法中辅料蔗糖用量和温度控制提供依据；参考世界卫生组织（WHO）及《中国居民膳食指南》中游离糖的控制指标，评估参麦颗粒中辅料蔗糖的每日摄入量，为患者健康提供指导。方法 采用HPLC测定30批参麦颗粒的糖类成分（果糖、葡萄糖、蔗糖）含量，计算游离糖的每日摄入量及供能比；采用Adobe Photoshop对来自同一光源下的参麦颗粒进行色度值（L^*、a^*、b^*）的测定，对色度值及糖类成分进行相关性分析、聚类分析及偏最小二乘法-判别分析（PLS-DA）。结果 参麦颗粒各厂家辅料蔗糖用量均超过处方规定量，相关性分析结果显示果糖和葡萄糖的含量与色度值L*呈极显著负相关，与a^*呈极显著正相关；可根据参麦颗粒颜色初步判断果糖和葡萄糖的含量，颜色越深，颗粒越偏红、偏蓝，含量越高。30批样品按不同厂家分别聚为三类，表明不同厂家生产的参麦颗粒颜色和糖类成分含量有差异显著，颜色越深，蔗糖降解越严重。30批参麦颗粒样品的蔗糖供能比均超过世界卫生组织（WHO）及《中国居民膳食指南（2022）》中建议的10%，建议厂家开发无糖剂型。结论 所建立的糖类含量测定方法准确稳定，重复性好，为处方制法合理性提供参考，为制粒过程温度控制提供依据；通过控制蔗糖日摄入量，为患者健康状况提供指导。     

HPLC测定转化糖注射液中果糖、葡萄糖含量

目的 建立转化糖注射液中果糖、葡萄糖的含量测定方法。方法 色谱柱为Hamilton HC-75H(305 mm×7.8 mm,9 μm),流动相为0.04 mol·L^-1磷酸,流速为0.5 mL·min^-1,检测波长为200 nm,柱温为50 ℃。结果 果糖和葡萄糖的检测限分别为0.28,0.52 μg;线性范围分别为1.27~3.81 mg·mL^-1(r=0.999 4)、1.26~3.76 mg·mL^-1(r=0.999 2);加样回收率分别为100.8%,100.4%。结论 本法适用于转化糖注射液中果糖、葡萄糖的含量测定。     

离子色谱法测定小儿复方氨基酸注射液中的氨含量

目的 采用离子色谱法优化测定小儿复方氨基酸注射液中的氨含量。方法 采用阳离子交换色谱柱RFICTM IonPac^® CG16（4 mm×50 mm）,保护柱CS16（4 mm×250 mm）;以20 mmol·L^-1甲基磺酸为流动相A,以100 mmol·L^-1甲基磺酸为流动相B,梯度洗脱,流速为1.0 mL·min^-1;检测器为电导检测器（带抑制器CERS 300,4 mm）;进样体积25 μl。结果 氨的线性范围为0.149 9~5.997 9 μg·ml^-1（r=0.998 4）,平均回收率为96.8%,RSD为2.82%。结论 该法专属性高、结果准确可靠,可用于小儿复方氨基酸注射液中氨的含量控制。     

HPLC-ELSD测定红参、麦冬及其制剂中糖的含量

目的 建立同时测定红参、麦冬及其制剂参麦注射液中果糖、葡萄糖、蔗糖、麦芽糖的含量。方法 采用Alltech Prevail Carbohydrate ES(4.6 mm×250 mm,5 μm)色谱柱,流动相为乙腈-水溶液(72∶28),流速：1.0 mL·min^-1,柱温：25 ℃,ELSD氮气压力：3.5 bar,漂移管温度40 ℃。结果 在确定的分析条件下,果糖、葡萄糖、蔗糖、麦芽糖分别在1.01~20.20 mg,0.48~9.66 mg,0.95~19.08 mg,0.96~19.28 μg内呈良好的对数线性关系,回收率均在95%~105%内。结论 该方法简便、准确、稳定,适合用于红参、麦冬及其制剂参麦注射液中各糖的含量测定。     

高效离子交换色谱法测定肌氨肽苷注射液中次黄嘌呤含量

目的 建立采用磺酸基阳离子交换键合硅胶的离子交换色谱法，对肌氨肽苷注射液中次黄嘌呤含量进行测定。方法 采用磺酸基阳离子交换键合硅胶色谱柱；水（硫酸调节pH值至2.5±0.1）为流动相；二极管阵列检测器，检测波长为260 nm；流速0.8 mL·min^-1；柱温30℃。结果 次黄嘌呤在1~50 μg·mL^-1线性良好，平均回收率为99.0%。结论 该方法操作简便，色谱图基线稳定，主成分峰形对称，分离度高，方法的重复性和耐用性好、准确度高，可用于肌氨肽苷注射液中次黄嘌呤的含量测定。     

不同产地桑叶氨基酸、核苷、生物碱成分的含量测定及多元统计分析

目的 建立超高效液相串联三重四极杆质谱（UPLC-TQD）同时测定桑叶样品中氨基酸、核苷及生物碱[1-脱氧野尻霉素（1-deoxynojirimycin，DNJ）]含量的方法，并采用多元统计分析方法分析比较不同产地桑叶中成分含量差异，为桑叶资源的品质评价提供科学依据。方法 采用Waters Acquity UPLC BEH Amide（100 mm×2.1 mm，1.7 μm）色谱柱，以0.2%甲酸乙腈（A）-0.2%甲酸水（B）梯度洗脱，流速0.4 mL·min^-1，柱温35℃；使用多反应监控正离子模式测定；采用多元统计分析如主成分分析对不同产地桑叶进行综合性评价。结果 22种成分的浓度与峰面积呈良好的线性关系（r² ≥ 0.990 3）；方法精密度、重复性及稳定性的RSD值均≤ 7.5%；平均加样回收率为86.7%~106.4%，RSD为2.2%~8.9%。不同产地桑叶中氨基酸、核苷及DNJ存在一定差异，结合多元统计分析，共找出8个差异性成分，可将样品分成2组。结论 所建立方法准确可靠，结合DNJ及8个差异性成分含量进行比较，湖北及江西产地的桑叶品质较优。     

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.