反相高效液相色谱法测定O／W型二氢青蒿素脂肪乳剂中二氢青蒿素含量

目的建立测定O／W型二氢青蒿素脂肪乳剂中二氢青蒿素含量的高效液相色谱法。方法采用AgilentHC—C18柱（250mm×4．6mm,5μm）,流动相为乙腈-水（60：40）,流速1．0mL／min,柱温25℃,检测波长216nm。结果该方法试样质量浓度0．002129-2．18g／L范围内与检测峰峰面积呈良好线性关系,平均回收率为95．33％,RSD=1．40％（n=9）。结论该方法简便、精密,回收率高,重现性好,可用于二氢青蒿素脂肪乳剂中二氢青蒿素含量的测定。     

RP-HPLC法测定黄花蒿中青蒿素含量

目的建立青蒿素的含量测定方法。方法采用HPLC外标法。色谱柱为C18柱(250mm×4.6mm,5μm);流动相为乙腈-水(45∶55);流速为1.0mL·min-1;检测波长为203nm;柱温为30℃。结果青蒿素对照品溶液在13.08～52.32μg的质量范围内与峰面积线性关系良好,r=0.9988,平均回收率为100.4%,RSD为0.9%(n=5)。结论该方法可用于青蒿素的含量测定。     

HPLC测定青蒿素原料药的含量并检查有关物质

目的 建立直接测定青蒿素原料药的含量和检查有关物质的方法.方法 采用HPLC法,色谱柱为Agilent C18柱,流动相为乙腈-水(65:35),流速1 ml·min-1,检测波长205 nm.结果 青蒿素进样量6.0～50.0μg与峰面积的线性关系良好(r=0.9999,n=6),平均回收率为100.1%,RSD=1.3%.结论 所用方法可用于青蒿素含量的测定及有关物质的检查.     

FMOC-Cl柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量

目的:建立氯甲酸-9-芴甲酯(FMOC-Cl)柱前衍生化HPLC法测定注射用帕米膦酸二钠的含量。方法:碱性条件下供试品与FMOC-Cl进行衍生化反应,采用Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈-0.4%EDTA溶液(用1 mol·L-1氢氧化钠溶液调节pH至7.2)(25∶75),流速1 mL·min-1,检测波长为265 nm。结果:帕米膦酸二钠浓度在0.05～1.00 mg·mL-1范围内与峰面积呈良好关系(r=0.9998),平均回收率为101.0%(n=9)。结论:该方法专属性好,适合用于注射用帕米膦酸二钠的含量测定。     

柱前衍生高效液相色谱法测定视明注射液中麝香酮含量

目的:建立将2,4-二硝基苯肼与视明注射液进行柱前衍生化反应,以 HPLC-UV 测定的分析方法。方法:使用江苏淮阴精化 C_(18)(4.6 mm×200 mm,5μm)色谱柱;乙腈-水(90∶10)为流动相,流速:1.0 mL·min~(-1);检测波长为365 nm。结果:麝香酮在1.60～7.00μg范围内线性关系良好,r=0.9997;平均回收率(n=3)为97.5%,RSD=1.6%。结论:该方法专属性强,灵敏准确,重现性好,为视明注射液的质量控制提供了有效的检测手段。     

HPLC-UV-ELSD联用测定黄花蒿叶片中青蒿素及相关倍半萜的含量

目的HPLC-UV-ELSD联用建立黄花蒿叶片中青蒿素及其生合成相关倍半萜的含量测定方法。方法采用Venusil XBP-C18色谱柱(200 mm×4.6 mm,5μm),流动相:乙腈-水梯度洗脱,检测波长:203 nm,流速:1.0 mL.min-1,ELSD载气压力:0.35 MPa,喷嘴温度:35℃,漂移管温度:60℃,检测器:UV-ELSD联用,测定黄花蒿叶片中青蒿素、青蒿素B、3α-羟基-1-去氧青蒿素含量。同一色谱柱条件下流动相改为乙腈-水-甲酸(体积比为60.00∶40.00∶0.08),检测波长:215 nm,流速:1.0 mL.min-1,检测器:UV检测器,测定黄花蒿叶片中青蒿酸含量。结果4种倍半萜在各自的线性范围内线性关系良好(r≥0.9990),RSD<3%,平均加样回收率分别为98.5%(RSD=2.3%)、96.5%(RSD=1.8%)、97.5%(RSD=3.6%)、95.4%(RSD=2.5%)。结论该方法可作为黄花蒿中青蒿素及其生合成相关倍半萜的含量测定方法。     

UV法与HPLC法测定青蒿中青蒿素含量的比较

目的:分别以高效液相色谱(HPLC)法与紫外分光光度(UV)法测定青蒿中青蒿素的含量,比较2种方法分析结果的差异。方法:HPLC法中色谱柱为Kromasil ODS C18(250mm×4.6mm,5μm),流动相为甲醇-水(75:25),流速为1.0mL·min-1,检测波长为203nm,柱温为30℃。UV法中样品溶液用0.2%NaOH衍生后,在292nm波长处测定。结果:HPLC法标准曲线的线性范围为0.025～0.400mg·mL-1(r=0.9999),平均加样回收率为97.18%(RSD=3.58%,n=9);UV法标准曲线的线性范围为4～20μg·mL-1(r=0.9998)。UV法含量测定结果比HPLC法平均高出2.05倍。结论:HPLC法的精密度、稳定性、加样回收率都较好,对青蒿中青蒿素含量的分析较为准确。UV法不宜单独用于青蒿中青蒿素的含量分析。     

高效液相色谱法测定黄杨宁片中环维黄杨星D的含量和含量均匀度

目的:建立 HPLC 测定黄杨宁片中环维黄杨星 D 含量和含量均匀度的方法并进行方法学验证。方法:采取异氰酸苯酯柱前衍生化,HPLC 测定。色谱柱:Lichrospher C_(18)(5μm,4.6 mm×250 mm);流动相:甲醇-水(83:17);流速1 mL·min~(-1);检测波长:240 nm;柱温:30℃。结果:线性范围在0.08624～0.4312μg(r=0.9999);测得环维黄杨星 D 的平均回收率为97.92%,精密度,重复性,线性关系良好,结论:该方法可靠、准确、灵敏度高,为黄杨宁片剂的质量控制建立了良好的方法。     

柱前衍生HPLC法测定体外培育牛黄中主要胆汁酸类成分北大核心CSCD

目的:建立体外培育牛黄样品溶液柱前衍生化处理后使用HPLC-UV进行测定的方法。方法:2-溴-4′-硝基苯乙酮和18-冠醚-6作为衍生化反应试剂,采用Agilent Zorbax SB-C_(18)(150 mm×4.6 mm,5μm)色谱柱,以水为流动相A,甲醇为流动相B,梯度洗脱,流速1 mL·min^(-1),在263 nm波长处进行测定,柱温为30℃。结果:胆酸和去氧胆酸进样量分别在0.25~4.00和0.20~3.21μg范围内线性关系良好;回收率分别为95.13%和94.87%,RSD(n=6)分别为2.09%和3.15%。3批样品的胆酸含量分别为7.3%、8.4%、8.1%,去氧胆酸含量分别为4.9%、5.6%、5.4%。结论:该法经方法学验证,适用于体外培育牛黄中主要胆汁酸类成分的含量测定。     

HPLC法测定L-谷氨酰胺及其胶囊剂的含量

目的:建立HPLC法测定L-谷氨酰胺及其胶囊剂的含量。方法:用DNFB进行柱前衍生化,以乙腈-0.01m01·L~(-1)磷酸二氢钾溶液(15:85)为流动相,检测波长为360nm。结果:测得线性范围12.82～128.2μg·ml~(-1)(r=0.9999),平均回收率为99.2％,RSD为0.85％(n=6)。结论:本法简便,快速,重现性好。     

Sterile Filtration of a Parenteral Emulsion

The Syntex adjuvant formulation (SAP) containing [thr¹]-muramyldipeptide in an oil-in-water emulsion has proven to be an effective adjuvant eliciting both cell-mediated and humoral immune response. As a parenteral emulsion, sterility of the final product was a concern, and various methods of achieving sterility were considered. For emulsions, most conventional sterilization methods are not viable, requiring the more cumbersome technique of sterilizing individual components and assembling/manufacturing under sterile conditions. Emulsion vehicles were manufactured with various models in the Microfluidizer M110 series. All equipment examined was capable of reducing the average dispersed oil droplet size to approximately 160 nm, with varying size ranges. Operating at an internal equipment pressure of greater than 16,000 psi, with at least five cycles through the interaction chamber, the resulting emulsion had a narrow droplet size range distribution, with the largest droplets being small enough to enable sterile filtration. Under specific-manufacturing conditions, the adjuvant emulsion becomes easily filtered through a 0.22-µm cartridge filter, thus yielding a sterile end product. This is the first published example of emulsion sterilization being achieved by terminal filtration.     

雅皓乳膏治疗牙周炎60例临床疗效分析

目的　观察雅皓乳膏治疗牙周炎的临床疗效。方法　将 6 0名牙周炎患者分成实验组 (雅皓乳膏 )和对照组 (碘甘油 ) ,采用自身对照 ,观察用药前后临床症状和牙周指数的变化。结果　两组临床症状和牙周指数有显著性差异 (P<0 .0 5 )。结论　雅皓乳膏对牙周炎有一定的治疗效果且优于碘甘油。     

地塞米松棕榈酸酯脂肪乳注射液的制备

摘 要 目的：制备地塞米松棕榈酸酯脂肪乳注射液,并评价其理化性质。方法: 采用热熔乳化 高压均质法制备地塞米松棕榈酸酯脂肪乳注射液,并对脂肪乳的粒径分布、PdI、Zeta电位和微观形态进行评价;初步考察地塞米松棕榈酸酯脂肪乳注射液的稳定性。结果: 制备的地塞米松棕榈酸酯脂肪乳注射液的平均粒径为（215.1±38.2）nm,PdI 为0.218,Zeta电位为（-18.1±2.3）mV;经透射电镜观察显示,地塞米松棕榈酸酯脂肪乳呈球形,大小分布较为均匀;长期稳定性试验结果表明,地塞米松棕榈酸酯脂肪乳注射液在6个月内稳定性良好。结论:采用热熔乳化 高压均质法制备地塞米松棕榈酸酯脂肪乳注射液工艺简单易行,有望应用于工业化生产之中。     

注射用克拉霉素乳剂的制备及其体内外评价

目的制备克拉霉素乳剂并考察其刺激性和体内药物动力学行为。方法通过高压均质方法制备克拉霉素乳剂，并对其性质进行研究。以克拉霉素溶液剂为对照，观察了乳剂的刺激性和在大鼠体内的药物动力学行为。结果高压均质法制备克拉霉素乳剂，平均粒径为156 nm，zeta 电位为-31.8 mV。于4 ℃留样观察6个月内样品稳定。与克拉霉素溶液剂相比，乳剂可以明显降低刺激性。两种制剂在大鼠体内的药物动力学曲线相似，符合双隔室模型。克拉霉素乳剂和溶液剂AUC0-t分别为(66.76±16.34)和(59.00±11.20) μg·h·mL^-1。结论高压均质法可以制备出性质稳定的载药乳剂，克拉霉素乳剂可以明显降低静脉注射时引起的刺激性。     

抗白内障药双硫伦乳剂的化学稳定性考察

考察了抗白内障药双硫伦乳剂中双硫伦的化学稳定性 ,测定了不同的乳剂组成对双硫伦化学稳定性的影响 ,得出双硫伦降解服从一级反应 ,速率常数与温度关系符合阿累尼乌斯方程 ,其中较好的处方中双硫伦于 4℃时的降解速度常数为 1 516× 10 -4·d-1 ,活化能为 153 2kJ·mol-1 ,t0 9,4℃为 695 2d     

月桂酸维生素C酯的表面活性和抗氧化性的研究

目的考察月桂酸维生素C酯 (DAC)的表面活性和抗氧化性。方法通过测定DAC的亲水亲油平衡值 (HLB)和临界胶束浓度 (cmc)考察DAC的表面活性 ;以DAC和吐温 - 80为乳化剂 ,邻苯三酚为模型化合物 ,制备O/W型乳剂 ;用终止邻苯三酚自氧化的方法考察DAC在水溶液和乳剂中的抗氧化性。结果HLB为 5 4 ,cmc为 7× 10 -5～ 8× 10 -5mol·L-1,O/W型乳剂稳定性良好 ,在溶液和乳剂中DAC均具有抗氧化能力 ,其抗氧化能力与其用量有关。结论DAC具有表面活性和抗氧化性 ,在乳剂中既能作为乳化剂同时又可作为抗氧剂     

注射用克拉霉素乳剂稳定性及影响因素考察

目的考察克拉霉素乳剂稳定性及其影响因素。方法以乳剂粒径,pH值变化和药物含量作为指标,考察了不同温度对克拉霉素乳剂稳定性的影响。结果乳剂在低温保存时稳定性良好,温度升高会显著影响乳剂稳定性,导致粒径增大和pH降低。根据Arrhenius公式求得储存温度为5℃时,T0.9=9.06年,长期稳定性试验结果表明,载药乳剂在12个月理化性质稳定。结论低温保存有利于提高该乳剂的稳定性。     

Cytosolic delivery via escape from the endosome using emulsion droplets and ultrasound

Vaporizing emulsion droplets may aid in endosomal rupture as a drug delivery route to the cytosol. Upon insonation, emulsion droplets formed from perfluorocarbon liquids may vaporize with sufficient expansion to disrupt liposomal or endosomal membranes. Emulsion droplets of perfluorohexane (PFC6) or perfluoropentane (PFC5) were prepared as free droplets in calcein or as droplets encapsulated within liposomes containing calcein. Folate-stimulated endocytosis created an experimental model, wherein calcein was self-quenched until released from the vesicles. Upon release, calcein was diluted below its self-quenching concentration and its release quantified by fluorescence. In this experimental model, folated emulsions or folated eLiposomes were incubated with folate-starved HeLa cells. Samples were exposed to two seconds of 20-kHz ultrasound (US) at 1?W/cm². Fluorescence microscopy identified released intracellular calcein. Upon insonation, both free emulsion samples and eLiposome samples produced calcein release to the cytosol. Calcein fluorescence was more intense in samples containing PFC5 compared to PFC6. Insonation of samples without emulsion droplets produced no cytosolic delivery. Likewise, cells that took up emulsion droplets but were not exposed to US did not exhibit fluorescence throughout the cell. These results suggest that vaporizing emulsion droplets are internalized into the cells and can produce endosomal escape of a therapeutic payload.     

O/W型甲苯咪唑混悬乳剂稳定性考察

以均匀设计法筛选检查甲苯咪唑降解产物的薄层色谱法,结果选择氯访-甲醇-甲酸（90：8：2）为展开系统;采用离心试验、留样观察法,光加速,热加速及温加过试验考察甲苯咪唑乳剂的物理、化学稳定性,结果表明该乳剂唯不耐60℃以上高温,室温下有效期为4.22年。     

Validation of Fiber-Optic Doppler Anemometry (FODA) for Characterizing the Droplet Size of Emulsions

Fiber-optic Doppler anemometry (FODA) is a useful tool to characterize polydisperse systems such as emulsions. The mean droplet radius of a model emulsion determined by FODA matched the mean radius determined by sizing droplets from a freeze-fractured freeze-etched scanning electron photomicrograph. The mean droplet radius determined by the Coulter technique was four times too large because the small droplets were not detected. The utility of FODA was further illustrated by its ability to accurately size droplets and monitor the coalescence upon aging of an intravenous lipid emulsion.