高效液相色谱-电感耦合等离子体质谱法测定海鱼中无机砷

目的建立测定海鱼中无机砷含量的高效液相色谱-电感耦合等离子体质谱法。方法海鱼样品经稀硝酸超声热水浴提取后,AS7阴离子交换色谱柱分离,3.5 mmol/L(NH4)2CO3+1%甲醇与100 mmol/L(NH4)2CO3+1%甲醇流动相梯度洗脱,电感耦合等离子体质谱仪测定,以保留时间定性,外标法定量。结果在1~100μg/L的线性范围,6种砷形态化合物的回归方程均呈良好的线性关系,相关系数均优于0.9996,检出限为0.05~0.25μg/L,定量限为0.17~0.84μg/L,3个浓度加标回收率为88.5%~106.4%,相对标准偏差为2.5%~4.9%。结论本方法满足海鱼中无机砷含量的测定要求,提取快速,稳定,操作简单,检出限低,方法的重现性好,灵敏度高。     

复方补血胶囊中葡萄糖酸亚铁的含量测定

目的：复方补血胶囊中葡萄糖酸亚铁的含量测定。方法：根据Fe^2 与邻二氮菲显色,在510nm处有最大吸收,利用分光光度法测定。结果：葡萄糖亚铁在7－34μg/ml的浓度范围内线性关系良好（r=0.9999),回收率、日内变异均符合要求,结论：建立了复方补血胶囊中葡萄糖酸亚铁的含量测定方法。     

东亚钳蝎蝎毒的指纹图谱

目的 :探索东亚钳蝎蝎毒 (scorpionofButhusmartensiivenom)的分析及鉴定方法 ,建立相关质量标准。方法 :采用高效液相色谱法 (highperformanceliquidchromatography ,HPLC)分析检测 8个蝎毒样品。结果 :蝎毒可分离出40多个组分 ,实验所使用的 8个省内所产蝎毒具有非常相似的图谱。蝎淋巴液和 3种蛇毒与蝎毒图谱有显著不同。同一样品 (二次冻干粉 )连续测定 5次进样量的精密度、重现性均达到有关规定。结论 :采用HPLC法获得了蝎毒的指纹图谱 ,并测定了可影响蝎毒质量的蝎淋巴液和可能用于掺伪的 3种蛇毒的图谱。本研究为蝎毒及其制剂的进一步开发应用提供了有价值的实验依据。     

热力学模型对石油低压汽液平衡计算的适用性

以Maxwell-Bonnel图拟合式、对比态Antoine方程及Pitzer-Riedel关联式分别求算饱和蒸汽压P^0,并用RoultK值（K＝P^0／P）,计算窄留分K值。根据实测的中原、孤岛和克拉玛依石油馏分低压K值,考察上述三式,结果表明：对比态Antoine式预测精度是最好的,其温度预测绝对平均偏差为7．0℃,K值预测平均相对偏差为15．6％,其他两模型偏差均较大。     

反相高效液相色谱分析胺甲硫磷和甲基毒死蜱的方法研究

建立了生物组织中胺甲硫磷和甲基毒死蜱的反相高效液相色谱分析方法。选用YWG-C18H375mm(内径)×200mm柱作为分析柱,流动相选用80∶20（V/V）的甲醇/水二元体系,流速为1.0ml/min,检测波长胺甲硫磷为252nm,甲基毒死蜱为290nm。该方法简单、快速、准确。其最小检出量为2.5×10-8g,最小检出浓度为0.25mg/L。     

创伤性脊髓损伤患者血清和尿液的代谢组学分析

背景:创伤性脊髓损伤在临床上主要依赖于量表评估与影像学检查,但对于损伤程度的预后评估具有一定局限性,利用代谢组学技术进行生物标志物筛选,对于估计病变范围、损伤与恢复程度以及开发新疗法具有重要意义。目的:使用代谢组学技术来表征创伤性脊髓损伤患者的代谢特征,探寻潜在的生物标志物及失调的代谢途径。方法:收集20例创伤性脊髓损伤患者(观察组)和10例健康受试者(对照组)的血清和尿液样本,进行代谢物分析,然后利用多元变量统计分析进行数据处理,筛选差异代谢物。通过MetaboAnalyst软件进行代谢通路富集,应用logistic回归构建生物标志物组合模型,并分析其与美国脊髓损伤协会(ASIA)分级的关系。结果与结论:两组受试者的血清和尿液中分别检测出160种和73种具有显著差异的代谢物。通路富集分析显示,创伤性脊髓损伤后脂质代谢出现明显的紊乱,包括鞘脂类、亚油酸、α-亚麻酸和花生四烯酸代谢以及糖基磷脂酰肌醇生物合成。识别出他索沙坦和葫芦素糖苷这组生物标志物,并且二者构成的代谢物组合在血清和尿液中的水平与ASIA分级存在相关性。由此可见,代谢组学技术为进一步理解创伤性脊髓损伤病理机制、筛选治疗靶点提供帮助。识别出的代谢生物标志物组合可能为评估创伤性脊髓损伤的严重程度提供参考。     

大剂量萘哌地尔在家犬体内的药物动力学

目的 :建立HPLC测定家犬血浆中萘哌地尔浓度的方法 ,研究大剂量萘哌地尔胶囊在家犬体内的药物动力学。方法 :健康家犬 5只 ,单剂量给予萘哌地尔胶囊 2 0 0mg后 ,在不同时间点从后肢静脉取血 ,血浆样品碱化后经乙醚提取 ,以乙腈 :磷酸盐缓冲液 (pH 6 .5 ) (6 0 :40 )为流动相 ,由ODSC18分析柱分离测定 ,紫外 2 30nm为检测波长 ,维拉帕米为内标。血药浓度数据用 3p97药物动力学程度处理。结果 :线性范围为 10～ 12 0 0ng·ml-1;方法回收率为98 83%～ 10 1 5 0 % ;日间RSD≤ 5 5 6 % ,日内RSD≤ 3 30 %。单剂量给予家犬萘哌地尔胶囊 2 0 0mg后 ,血药浓度随时间变化规律符合一室开放模型 ,T1/2Ke为 1 91～ 4 99h ,Tmax为 1 87～ 3 2 1h ,Cmax为 338 79～ 414 0 4ng·ml-1。结论 :本方法简便、回收率高、重现性好 ,用于大剂量萘哌地尔在动物体内的药物动力学研究 ,切实可行。     

HPLC analysis of 16 compounds from Artemisia ordosica

Objective: To establish a high-performance liquid chromatographic method (HPLC) for the simultaneous determination of sixteen compounds from Artemisia ordosica. Methods: HPLC was used to analyze 16 quality indicators of A. ordosica. The HPLC conditions were as follows: Agilent Eclipse Plus C18 column (250 mm × 4.6 mm, 5 μm) with acetonitrile (A)-water (B) as mobile phase, gradient elution: 0?10 min, 75%?65% B; 10?30 min, 65%?35 % B; and finally 30?40 min, 35%?15% B. The flow rate was 1.0 mL/min, the column temperature was 40 °C, the injection volume was 10 μL, and monitored by absorbance at 285 nm for compounds 1?10, 12 and 225 nm for compounds 11, 13?16. Results: Under the selected experimental chromatographic conditions, compounds 1?16 showed good linearity (r > 0.9993) in a wide concentration range. Their average recoveries were 99.50%, 95.38%, 97.75%, 96.00%, 98.20%, 97.50%, 95.50%, 99.33%, 96.75%, 96.50%, 98.50%, 97.83%, 99.20%, 95.33%, 97.33% and 96.30%, respectively, and the RSD were 1.99%, 1.81%, 1.63%, 1.98%, 1.67%, 1.92%, 1.74%, 1.67%, 1.90%, 1.72%, 1.88%, 1.83%, 1.79%, 1.76%, 1.81% and 1.96%, respectively. Conclusion: Based on the results of the HPLC analysis, it was concluded that p-hydroxycinnamic acid (1), O-hydroxycinnamic acid (2), coniferyl alcohol (5), 5,4''-dihydroxy-7,3''-dimethoxyflavanone (8), 5,4''-dihydroxy-7-methoxyflavanone (9), 5-hydroxy-7,4''-dimethoxyflavanone (12), dehydrofalcarindiol (13), arteordoyn A (14), dehydrofalcarinol (15) and capillarin (16) are best suited for the role of quality indicators of A. ordosica grown in different ecological environments.     

Salvage of pyrimidine nucleosides by Trichomonas vaginalis

Trichomonas vaginalis is incapable of de novo pyrimidine biosynthesis because it cannot incorporate bicarbonate, aspartate or orotate into its pyrimidine nucleotides or nucleic acids. The organism can salvage exogenous cytidine greater than uridine greater than uracil and thymidine, and incorporate them into the nucleotide pool. A portion of cytidine is converted to CMP, CDP and CTP by cytidine phosphotransferase and nucleotide kinases. Some cytidine and most of uracil are, however, converted first to uridine by cytidine deaminase and uridine phosphorylase respectively; uridine is then incorporated into UMP, UDP and UTP by uridine phosphotransferase and nucleotide kinases. The two phosphotransferases, found mainly in the non-sedimentable fraction of T. vaginalis, provide the main avenue of pyrimidine salvage. No significant levels of pyrimidine phosphoribosyl transferase or nucleoside kinases can be detected in the extract. T. vaginalis has no appreciable dihydrofolate reductase or thymidylate synthetase; it grows normally in millimolar concentrations of methotrexate, pyrimethamine, or trimethoprim, and cannot incorporate labels from exogenous uracil or uridine into DNA. It has an enzyme thymidine phosphotransferase in the sedimentable fraction which converts thymidine to TMP. Thymidine salvage in T. vaginalis is thus totally isolated from the rest of the pyrimidine salvage.     

Distribution of neuropeptide Y in the prosencephalon of man and Cotton-head Tamarin (Saguinus oedipus): colocalization with somatostatin in neurons of striatum and amygdala

Summary The presence, chromatographic properties and localization of neuropeptide Y was demonstrated in postmortem human brain areas of neurologically and neuropsychiatrically normative controls using immunocytochemistry and high performance liquid chromatography combined with radioimmunoassay. NPY-immunoreactivity was found in many regions of the prosencephalon. Numerous perikarya and fibers were present in the neocortex, basal ganglia and limbic-hypothalamic areas. A moderate number of neurons and fibers was observed in the basal forebrain, including the septal complex. A comparative immunohistochemical investigation in perfusion-fixed brains of the old-world ape Saguinus oedipus revealed an almost identical distribution of NPY-immunoreactivity with only minor differences. Colocalization experiments on 1–2 m thin consecutive paraffin sections revealed a large number of NPY neurons throughout the human neostriatum and amygdaloid complex that were also positive for somatostatin. Our findings indicate that detection of neuropeptides in fresh or fixed post-mortem human tissue by different immunochemical methods may actually reflect the in vivo conditions. In addition, the wide distribution of NPY throughout the human brain and its colocalization with other neurotransmitters suggests a physiological role as neuroactive substance, i.e. neuromodulator in the primate central nervous system.