肝脏血液灌流中活性炭用量对阿霉素吸附效果的影响

目的以活性炭作为吸附剂,确定阿霉素在血液灌流法治疗肝癌时所用吸附剂的最佳用量,以减少阿霉素的毒副作用。方法采用含阿霉素的血浆灌注于不同组合量的活性炭柱,用柱切换高效液相色谱法测定阿霉素的灌注前后血药浓度。结果A组(150g×1支)、B组(150g×2支)、C组(150g×3支)、D组(150g×4支)及E组(150g×5支)活性炭柱对阿霉素的吸附率分别为20.19%、27.60%、55.98%、56.42%、57.13%,经方差分析有极显著性差异,经两两比较的q检验,C、D及E组间无显著性差异。结论除D组与E组P>0.05外,其它三个低剂量活性炭组中任意两组皆为P<0.01,故150g×3支活性炭柱为活性炭吸附剂的最佳用量,该用量的确定为血液灌流法治疗肝癌提供了理论依据。     

柱切换LC-MSn法分析阿莫西林钠克拉维酸钾原料的杂质谱#br#

目的 对阿莫西林钠克拉维酸钾复方原料中的杂质结构进行分析。方法 采用BDS Hypersil C18色谱柱,以0.01mol/L 磷酸二氢钾溶液(pH6.0)-乙腈为流动相进行梯度洗脱分离杂质;对阿莫西林钠克拉维酸钾(5:1)原料进行强力实验,归属杂质来源;采用柱切换-LC/MSn技术采集杂质的质谱数据,根据青霉素类抗生素的质谱裂解规律和降解反应机理,推定相关杂质的化学结构。结果 在原料中共检出并推断出11种杂质的化学结构,均为阿莫西林相关杂质,未检出与克拉维酸钾相关的杂质。结论 采用柱切换-LC-MSn技术可快速推定阿莫西林钠克拉维酸钾复方原料中相关杂质的化学结构,为《中国药典》中该类药品标准的提高提供了基础数据。     

基于全身免疫炎症指数的预测帕金森病患者伴发抑郁的列线图模型构建

目的 探讨全身免疫炎症指数(SII)与帕金森病(PD)患者发生抑郁的关系及其预测价值。方法 选取2017年1月至2022年12月徐州医科大学附属淮安临床学院收治的PD患者146例为PD组,同期于该院体检的健康者160例为对照组。根据汉密尔顿抑郁量表24项(HAMD-24)评分将PD组患者分为PD不伴抑郁组(n=77)、PD轻度抑郁组(n=51)、PD中重度抑郁组(n=18)。收集各组一般资料及实验室资料,采用多因素Logistic回归分析筛选PD患者发生抑郁的影响因素,并据此构建列线图预测模型。结果 PD组淋巴细胞计数和血小板计数均低于对照组,SII高于对照组(P<0.05)。PD不伴抑郁组、PD轻度抑郁组、PD中重度抑郁组3组间的左旋多巴等效剂量(LED)、病程、SII、H-Y分期、统一帕金森病评定量表第三部分(UPDRSⅢ)评分比较,差异有统计学意义(P<0.05)。多因素Logistic回归分析结果显示,较高的SII和UPDRSⅢ评分是PD患者发生抑郁的独立危险因素。基于SII及UPDRSⅢ评分构建的列线图模型的ROC曲线显示,SII诊断PD患者发生抑郁的AUC为0....     

藏边大黄的化学成分研究

目的 研究蓼科波叶组藏边大黄的化学成分.方法 采用硅胶、聚酰胺和ODS柱层析法.结果 分离得到11个化合物,经化学方法和波谱学鉴定,确定结构分别为:大黄酚(Ⅰ)、大黄素甲醚(Ⅱ)、大黄素(Ⅲ)、β-谷甾醇(Ⅳ)、trans-3,5,3′,4′-四羟基芪(Ⅴ)、d-儿茶素(Ⅵ)、胡萝卜苷(Ⅶ)、trans-3,5,3′,4′-四羟基芪-4′-O-β-D-吡喃葡萄糖苷(Ⅷ)、trans-3,5,3′,4′-四羟基芪-4′-O-β-D-(6″-O-没食子酰)-吡喃葡萄糖苷(Ⅸ)、大黄素-8-O-β-D-吡喃葡萄糖苷(X)和大黄酚-8-O-β-D-吡喃葡萄糖苷(Ⅺ).结论 其中Ⅸ系首次从该植物中分得.     

乳癖宁贴膏质量控制方法研究

目的:建立乳癖宁贴膏的质量控制方法。方法:采用薄层色谱法对乳癖宁贴膏中淫羊藿、土贝母、川楝子进行定性鉴别;采用柱层析-高效液相色谱法对其中君药淫羊藿进行含量测定。结果:在薄层色谱中均能鉴别出淫羊藿、土贝母、川楝子;淫羊藿苷进样量在0.428μg～2.568μg范围内与峰面积积分值线性关系良好(r=0.9998);平均加样回收率为94.57%(RSD=1.43%)。结论:本方法灵敏、准确、重现性好,可用于本品的质量控制。     

急性胰腺炎并发全身炎症反应综合征列线图预测模型的构建

目的 分析急性胰腺炎（AP）病人并发全身炎症反应综合征（SIRS）的风险因素,构建的列线图预测模型。方法 回顾性分析西南医科大学附属医院2020年4月至2022年4月收治的370例AP病人的临床资料,用于建模及内部验证,根据病人是否合并SIRS分为非SIRS组（n=273）和SIRS组（n=97）,通过logistic回归分析确定并发SIRS的独立危险因素,同时建立列线图可视化预测模型,计算一致性指数（C-index）,检验模型准确性;并探讨列线图模型对AP病人发生SIRS的预测效能。结果AP病人合并SIRS发生率为26.2%;白细胞计数、心率、并发胸腔积液为AP病人并发SIRS的危险因素（OR>1,P<0.05）;男性、高密度脂蛋白胆固醇（HDL-C）为AP病人并发SIRS的保护因素（0相似文献   

Fixed-bed column study for removal of phenol by neem leaves – Experiment,MLR and ANN analysis

This research aims to carry out the column study to remove toxic phenol by natural adsorbent neem leaves (Azadirachta indica). The adsorbent was characterized through SEM, XRD, FTIR, and BET. The phenol removal was performed in the fixed-bed column at optimum pH 3 and room temperature with the change of process variables, i.e., bed height (8.5–13.5 cm), flow rate (10–30 ml/min), and phenol content (100–300 mg/L). These experiments revealed that the breakthroughs of phenol occurred faster for lesser bed height, higher flow rate, and higher phenol content. The Yen et al. model is the best fitted kinetic model and is applicable for scale-up design. The DFT shows that the interaction between different components of the adsorbent and phenol. The artificial neural networks (ANN) modeling using a single hidden layered neural network is successful with the Levenberg-Marquardt algorithm. Desorption of phenol and safe disposal from the used adsorbents were reported.     

Temperature and eluent composition effects on enantiomer separation of carvedilol by high-performance liquid chromatography on immobilized amylose-based chiral stationary phases

Carvedilol is a chiral drug with potent antihypertensive and antianginal activities. Although it is clinically used as a racemic mixture, its enantiomers show different pharmacokinetic and pharmacodynamic profiles. Here, the direct chiral separation of racemic drug by high performance liquid chromatography using two immobilized-type amylose-based chiral stationary phases is presented. Some chromatographic parameters, such as retention and selectivity, were determined under multimodal eluent conditions and different temperatures. A temperature-dependent inversion of the elution order of enantiomers was observed in the operative temperature range of chiral chromatographic support. Finally, an effective direct enantioselective method was successfully applied to the separation of the enantiomers of carvedilol on a semipreparative scale.     

Recent advances in column switching high-performance liquid chromatography for bioanalysis

Bioanalysis is a relevant area of analytical chemistry for clinical studies. Biological samples are complex and diverse, so sample preparation represents a challenge when chromatographic methods are developed. According to the principles of green analytical chemistry (GAC), recent trends in sample preparation include miniaturization, automation (online coupling to the analytical instrument), and high-throughput performance. In this context, column switching liquid chromatography stands out as a multidimensional chromatographic method in which an extraction column is directly coupled to high-performance liquid chromatography (HPLC) systems. This online method consists of two steps and involves two columns, the extraction and the chromatographic columns. In the former column, the analytes are isolated from the sample and preconcentrated; in the latter column, the analytes are separated. Online systems improve the sensitivity and accuracy of analytical methods, consume lower amounts of organic solvents, and minimize sample handling. This review summarizes state-of-the-art column switching liquid chromatography and focuses on selective stationary phases for preconcentration of analytes (first dimension), including reversed phases, monolithic phases, restricted access materials (RAMs), and molecularly imprinted polymers (MIP). Principles, instrumental aspects, applications in bioanalysis, and future trends in column switching liquid chromatography are also discussed.     

CT based management of high energy tibial plateau fractures: A retrospective review of 53 cases

ObjectivesThe management of high energy tibial plateau fractures is a surgical challenge. Recently described Luo’s classification is based on CT scans and is more objective with a better inter-observer agreement as compare to Schatzker and AO/OTA classifications. We describe the functional results of a series of 53 cases classified and managed according to the Luo’s column concept.MethodsA retrospective review of 53 high energy tibial plateau fractures, operated between January 2012 and March 2015 at a Level I trauma center, was performed. CT scans were used to classify these injuries based on the number of columns involved. Plating configuration and surgical approach were chosen based on the number of independent articular fragments on axial sections at the level of fibular head.Results1 one-column, 51 two-column and 1 three-column fractures were studied. Triple plating was done in 5 patients. Mean follow-up was 2.7 years and mean Insall Knee score was 95.42. Four patients had varus malalignment and 1 had joint depression in the post-operative period. These were due to imperfect reduction during the surgery itself, and no case of late collapse was detected.ConclusionUtilizing Luo’s classification for treating these complex injuries will assist in better understanding of fracture pattern and hence help in achieving a better functional outcome. Each fractured column needs to be independently addressed.