GC测定褪黑素类似物中有机溶剂残留量

目的 建立毛细管气相色谱法测定褪黑素类似物AGO中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯5种有机溶剂的残留量。方法 采用DB-Wax(30 m×0.45 mm,0.85 μm)毛细管色谱柱;氢火焰离子化检测器(FID);程序升温：初始温度45 ℃(维持9 min),以30 ℃.min-1速率升温至200 ℃(维持9 min);载气为氮气,柱流速为3.5 mL.min-1;进样口温度：200 ℃;检测器温度：250 ℃;分流直接进样,二甲基亚砜为溶剂,乙腈为内标物,内标法测定残留溶剂的含量。结果 各组分分离完全,在所考察的浓度范围内线性关系良好,其中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯的线性范围分别为107.44 μg.mL-1~1074.4 μg.mL-1(r=0.9999),108.24 μg.mL-1~1082.4 μg.mL-1(r=0.9997),18.550 μg.mL-1~185.50 μg.mL-1(r=0.9998),14.208 μg.mL-1~142.08 μg.mL-1(r=0.9994),19.074 μg.mL-1~190.74 μg.mL-1(r=0.9999),平均回收率为98%~102%。结论 该方法操作简单,精密度好,准确可靠,可用于该药物有机溶剂残留量的测定。     

气相色谱法测定美洛昔康中有机溶剂残留量

目的 建立测定美洛昔康中有机溶剂残留量的方法.方法 气相色谱法,PEG-20M(30m×0.32mm,0.25μm)弹性石英毛细管柱,氢火焰离子化检测器,柱温:35℃(恒温5min),以10℃·min-1的升温速率至140℃(恒温2min);以20℃·min-1的升温速率至220℃(恒温5min).进样口温度:250℃;检测器温度:250℃;载气:氮气;进样方式:直接进样法;进样量:1μL.结果 4种溶剂的回收率在100.0%～101.5%之间,相对标准偏差均小于2%,最低检出限为1.0×10-3 μg·mL-1～5.0×10-3 μg·mL-1.结论 本方法准确、简便、快捷,可用于美洛昔康中的有机溶剂残留测定     

气相色谱法测定人血白蛋白中乙醇残留量

目的：建立气相色谱法测定人血白蛋白中乙醇残留量。方法：采用DB-624毛细管色谱柱（30 m×0.32 mm×1.8 μm）;氢火焰离子化检测器（FID）;进样口温度为200 ℃,检测器温度为250 ℃;载气为氮气,载气流速为2.0 mL·min-1;采用程序升温法：起始温度为40 ℃,保持8 min,以50 ℃·min-1速度升温至200 ℃,保持5 min。进样方式为顶空进样,顶空平衡温度为80 ℃,平衡时间为30 min。结果：乙醇在1.005 6 ~ 377.097 5 μg·mL-1范围内与峰面积线性关系良好（r为0.999 8,n=9）;精密度的RSD为2.5%,重复性的RSD为1.5%;平均加样回收率为100.2%（n=9,RSD为3.4%）。定量限为1.005 6 μg·mL-1,检出限为0.335 2 μg·mL-1。测定人血白蛋白原液59 批和成品78 批,均低于250 μg·mL-1。结论：该方法操作简单、结果准确,灵敏度高,专属性强,可用于人血白蛋白中乙醇残留量测定。     

气相色谱法测定鹿血酒中的甲醇和杂醇油

目的 建立气相法测定鹿血酒中甲醇和仲丁醇、正丙醇、正丁醇、异丁醇、异戊醇5种杂醇油成分.方法 Agilent HP-INNOWax(30 m×320 μm×0.25 μm)柱;程序升温;进样口温度230 ℃,进样量1 μL,分流比50∶1;氢火焰离子化检测器(FID),温度250 ℃;外标法定量.结果 鹿血酒中甲醇与5种杂醇油成分分离良好,在一定浓度范围内线性关系良好;加样回收率为91.6%~106.3%,定量限为2~11 μg·mL-1,检出限为1~6 μg·mL-1.结论 本法简便,准确,可用于鹿血酒中甲醇和5种杂醇油成分的含量测定.     

GC同时测定麝香通心滴丸中龙脑、异龙脑和麝香酮的含量

摘要：目的 建立同时测定麝香通心滴丸中龙脑、异龙脑及麝香酮含量的气相色谱法。方法 色谱柱：HP-5MS毛细管色谱柱(30 m×0.32 mm,0.25 μm),检测器为FID检测器,检测器温度为250 ℃,进样口温度220 ℃。柱温以100 ℃为初始温度,保持2分钟,以2 ℃?min-1升温至110 ℃,保持3分钟,以50 ℃?min-1升温至205 ℃,保持7分钟,以20 ℃?min-1升温至250 ℃,保持2分钟;载气为氮气,流速为1 mL?min-1;进样方式为分流进样,分流比为10：1;进样量为1 μL,以萘为内标。结果 龙脑、异龙脑、麝香酮的浓度分别在0.05468~0.4374 mg?mL-1(r=0.9999),0.07067~0.5654 mg?mL-1(r=0.9999),0.004512~0.03610 mg?mL-1(r=0.9997)的范围内线性良好;平均回收率分别为97.91 %(RSD=2.05 %),100.79 %(RSD= 2.78 %),105.36 %(RSD=3.78 %)。结论 该方法有效可靠,可用于麝香通心滴丸中龙脑、异龙脑和麝香酮的含量测定。     

聚维酮K90中三乙醇胺的测定

目的：建立药用辅料聚维酮K90中三乙醇胺的测定方法。方法：采用毛细管气相色谱法,以50%苯基-50%甲基聚硅氧烷为固定液(DB-17,30m×0.32mm,0.25μm),起始温度100℃,以10℃.min-1升温至240℃,保持2分钟,氢火焰离子化检测器,进样口温度260℃,检测器温度290℃,以氮气为载气,流速2mL.min-1,分流比10:1。结果：在选定的色谱条件下,三乙醇胺与内标邻苯二甲酸二乙酯分离良好,样品中的其他成分不干扰测定。以内标法计算,三乙醇胺线性回归方程为Y=0.024C-0.667(r=0.9995),线性范围36.2μg.mL-1～361.8μg.mL-1,平均回收率为95.0%(n=6),精密度为4.5%(n=6),检出限为12.1μg.mL-1,定量限为36.2μg.mL-1。3批聚维酮样品的三乙醇胺的含量均为0.2%。结论：该方法准确、可靠,可用于聚维酮K90中三乙醇胺残留测定,同时为聚维酮其他型号样品中三乙醇胺的测定提供依据。     

毛细管气相色谱法测定柠檬酸三乙酯含量

目的 建立毛细管气相色谱法测定柠檬酸三乙酯的含量.方法 色谱柱:DB-1301(15 m×0.53 mm×1 μm);柱温采用程序升温:先80℃保持0.5 min,然后以20℃·min-1的速度增加到220℃并保持10 min;采用氢火焰离子化检测器(FID),检测器温度:275℃;进样口温度:225℃;载气:氮气,流速:2.3 ml·min-1;分流比:20:1;进样量:1.0 μl.结果 柠檬酸三乙酯在24～36 g·L-1浓度范围内线性关系良好(r=0.999 17),平均回收率为99.91%,RSD值为0.06%.结论 该方法准确、简便、专属性强,可以作为柠檬酸三乙酯含量分析法.     

气相色谱法测定荧光素钠原料药中的残留溶剂

目的建立气相色谱法测定荧光素钠原料药中残留溶剂。方法选用毛细管柱DB-WAX(30.0m×0.25mm×0.25μm),氢火焰离子化检测器(FID),色谱条件:初温60℃(保持10min),以100℃·min-1升至200℃(保持1min),进样口温度:230℃,检测器温度:250℃。选择正丙醇作为内标,进样量1μL。结果二氯甲烷在(62.97~176.31)μg·mL-1浓度范围内与峰面积/内标峰面积比值呈良好的线性关系,检测限为25.19μg·mL-1,溶剂和内标对测定无干扰,3批样品均未检出二氯甲烷。结论经方法学验证,本方法简便灵敏,准确,可用于荧光素钠原料药中残留溶剂的检测。     

GC法同时测定冰珍去翳滴眼液中冰片和苯氧乙醇的含量

目的：建立气相色谱法同时测定冰珍去翳滴眼液中冰片及苯氧乙醇的含量。方法： 采用DB-WAX毛细管色谱柱（30 m × 0.32 mm,0.25 μm）;FID检测器;进样口温度200 ℃,检测器温度为250 ℃;载气为氮气,流速为1 mL·min-1。采用程序升温法：起始温度130 ℃,保持10 min,以25 ℃·min-1升至200 ℃,保持5 min。结果：天然冰片、苯氧乙醇的质量浓度分别在0.011 54～0.115 4 mg·mL-1（r=0.999 9）、0.064 87～0.648 7 mg·mL-1（r=0.999 9）范围内线性关系良好;平均回收率分别为96.3%（RSD=1.65%）、95.1%（RSD=1.62%）。结论：该方法专属性好,准确度高,重复性好,可用于冰珍去翳滴眼液的质量控制。     

GC法检测布洛芬注射液中杂质F

目的建立气相色谱法测定布洛芬注射液中的杂质F。方法采用气相色谱法,色谱柱：DB-WAXetr毛细管柱（25 m×0.53 mm×2μm）,载气为氦气,流速5.0 mL·min-1,检测器为火焰离子化检测器,检测器温度为250℃,进样温度为200℃。结果在选定的条件下布洛芬和杂质完全分离,杂质F的检测限为2.5 mg·L-1,检测方法的精密度、准确度、灵敏度均达到了预定的分析要求。结论建立的方法准确、灵敏,适用于检测布洛芬注射液中的杂质F。     

3,4-Methylenedioxymethamphetamine enhances the release of acetylcholine in the prefrontal cortex and dorsal hippocampus of the rat

Rationale The neurochemical effects produced by acute administration of 3,4-methylenedioxymethamphetamine (MDMA) on the monoaminergic systems in the brain are well documented; however, there has been little consideration of the potential effects of MDMA on other neurotransmitter systems. Objective The present study was designed to investigate the acute effect of MDMA on cholinergic neurons by measuring acetylcholine (ACh) release in the medial prefrontal cortex (PFC) and dorsal hippocampus, terminal regions of cholinergic projection neurons originating in the basal forebrain. Methods In vivo microdialysis and high-performance liquid chromatography with electrochemical detection (HPLC-ED) were used to assess the effects of MDMA on the extracellular concentration of ACh in the PFC and dorsal hippocampus of the rat. Results The systemic administration of MDMA (3–20 mg/kg, i.p.) resulted in an increased extracellular concentration of ACh in the PFC and dorsal hippocampus. Reverse dialysis of MDMA (100 μM) into the PFC and hippocampus also increased ACh release in these brain regions. Treatment with parachlorophenylalanine and α-methyl-para-tyrosine, inhibitors of serotonin (5-HT) and dopamine (DA) synthesis, respectively, significantly attenuated the release of ACh stimulated by MDMA in the PFC, but not in the dorsal hippocampus. Conclusions MDMA exerts a stimulatory effect on the release of ACh in the PFC and dorsal hippocampus in vivo, possibly by mechanisms localized within these brain regions. In addition, these results suggest that the MDMA-induced release of ACh in the PFC involves both serotonergic and dopaminergic mechanisms.     

Impact of sampling time deviations on the prediction of the area under the curve using regression limited sampling strategies

The regression limited sampling strategy approach (R‐LSS), which is based on a small number of blood samples drawn at selected time points, has been used as an alternative method for the estimation of the area under the concentration–time curve (AUC). However, deviations from planned sampling times may affect the performance of R‐LSS, influencing related therapeutic decisions and outcomes. The aim of this study was to investigate the impact of different sampling time deviation (STD) scenarios on the estimation of AUC by the R‐LSS using a simulation approach. Three types of scenarios were considered going from the simplest case of fixed deviations, to random deviations and then to a more realistic case where deviations of mixed nature can occur. In addition, the sensitivity of the R‐LSS to STD in each involved sampling point was evaluated. A significant impact of STD on the performance of R‐LSS was demonstrated. The tolerance of R‐LSS to STD was found to depend not only on the number of sampling points but more importantly on the duration of the sampling process. Sensitivity analysis showed that sampling points at which rapid concentration changes occur were relatively more critical for AUC prediction by R‐LSS. As a practical approach, nomograms were proposed, where the expected predictive performance of R‐LSS was provided as a function of STD information. The investigation of STD impact on the predictive performance of R‐LSS is a critical element and should be routinely performed to guide R‐LSS selection and use. Copyright © 2015 John Wiley & Sons, Ltd.     

LPS致热家兔诱导HSF1聚合对体温及脑内AVP含量的影响

目的探讨热休克因子1(HSF1)在脂多糖(LPS)致家兔发热过程中的作用及机制。方法70只家兔随机分为4组:正常对照组(N)、槲皮素组(Q)、脂多糖组(L)和槲皮素+脂多糖组(Q+L)。连续观察体温变化;Westernblot方法检测不同实验条件下下丘脑HSF1和热休克蛋白70(HSP70)的表达;放射免疫法检测下丘脑及腹中隔区(VSA)精氨酸加压素(AVP)含量的变化。结果①各组体温变化最大值(△Tmax)由低至高顺序为:Q组相似文献   

乙酰吉他霉素临床前药理学研究

乙酰吉他霉素对临床分离的革兰氏阳性球菌有较好的抑菌活力，其对金葡球菌、β－溶血性链球菌、表葡球菌的ＭＩＣ_（５０）分别为１、０．２２和４ｍｇ／Ｌ，对耐红霉素、青霉素的金葡球菌、表葡球菌半数以上较敏感，与吉他霉素相似，但其对革兰氏阴性菌无明显作用。乙酰吉他霉素对小鼠实验性细菌感染有明显保护作用。对金葡球菌、肺炎双球菌感染小鼠口服用药的ＥＤ_（５０）分别为７９．６和２５．１ｍｇ／ｋｇ。其疗效与吉他霉素、麦白霉素、乙酰螺旋霉素相似。乙酰吉他霉素小鼠１次口服的ＬＤ_（５０）＞１５ｇ／ｋｇ，与吉他霉素相比毒性无差异。     

硝苯地平固体分散体胶囊剂的制备

目的:将难溶于水的硝苯地平(nifedipine,NF)制成聚乙二醇4000(PEG4000)固体分散体胶囊剂,以改善其溶出性能.方法:①溶剂(乙醇)-熔融法制备硝苯地平-PEG4000固体分散体,并添加适宜稀释剂尿素(或甘露醇、蔗糖、柠檬酸、β-环糊精)制成胶囊;②正交设计确定PEG4000、稀释剂最佳用量;③量热分析法、溶出度法验证NF固体分散体.结果:①正交设计确定了PEG4000、稀释剂尿素最佳用量,溶剂-熔融法制得NF固体分散体.②工艺是将NF超声分散于乙醇(体积质量比1:24)中,加入熔融(70℃)的PEG4000(与NF的质量比1:4)中,使均匀混合,添加尿素(与NF的质量比1:20),80℃挥去乙醇,填充胶囊.③样品DSC曲线中NF熔融峰(177℃)消失,PEG4000峰(66℃)前移;胶囊均重0.25 g,含NF 10 mg,溶出t0 525～35 min.结论:溶剂-熔融法成功制备NF固体分散体,NF溶出度显著增大;添加尿素填充胶囊不影响固体分散体的溶解性;工艺简单、易行、成本较低.     

The effect of (+/-)mianserin and its enantiomers on the behavioural hyperactivity of the olfactory-bulbectomized rat

The effects of (+/-)mianserin and its enantiomers on the behavioural hyperactivity of the olfactory bulbectomized (OB) rat and on the levels of some central neurotransmitters were investigated. The reversal of hyperactivity by racemic mianserin was found to be independent of dose within a non-sedative range of 2-10 mg/kg and occurred following seven days of treatment. Chronic administration of racemic mianserin, over the dose range 2-15 mg/kg elevated the steady-state concentration of noradrenaline in the amygdaloid cortex and midbrain. Of the two enantiomers, only the behaviourally active (+)-(S)-form increased the steady state concentration of noradrenaline in these two areas of the brain. The reversal of the hyperactivity by (+/-)mianserin and the (+)-(S)-enantiomer was not associated with a change in the concentration of serotonin or 5-hydroxyindole acetic acid. The behaviourally inactive enantiomer (-)-(R) decreased the concentration of 5-hydroxyindole acetic acid, an effect which may be associated with the sedative action of the drug. The results suggest that the reversal of the behavioural hyperactivity of the olfactory bulbectomized (OB) rat by (+/-)mianserin and its (+)-(S)-enantiomer is associated with an increase in the steady-state concentration of noradrenaline, in the areas of the brain studied.     

防治痴呆新药的构效关系研究

阿尔茨海默病、帕金森病和血管性痴呆是严重危害老年人生命健康的多发病。目前临床应用的防治痴呆药物的作用机制主要涉及改善胆碱能神经递质、激动多巴胺(DA)受体、阻滞N-甲基-D门冬氨酸(NMDA)受体和改善脑血管功能等。综述了近年来报道的防治痴呆新药的构效关系研究进展。     

计算机X线摄影系统在胸外伤诊断中的作用

目的评价计算机X线摄影(CR)系统在胸外伤患者检查中的诊断价值。方法对80例胸外伤患者的胸部正位CR片与普通X线(CF)平片进行回顾性对比分析 ,比较二者在肋骨骨折、肺挫伤及血气胸诊断中的敏感程度和准确度。结果CR片发现肋骨骨折27例 ,血气胸5例 ,肺挫伤4例 ;普通X线平片发现肋骨骨折18例 ,血气胸4例 ,肺挫伤2例。经 χ2 检验 ,CR和CF对胸外伤患者胸部病变的敏感程度和准确度有显著差异(P<0.05)。结论CR系统在胸外伤患者胸部检查中具有更高的价值。     

ARB和ACEI维持性血液透析患者EPO疗效比较

目的：观察血管紧张素Ⅱ受体拮抗药（ARB）对维持性血液透析患者重组人红细胞生成素（EPO）疗效的影响，并与血管紧张素转换酶抑制药（ACEI）进行比较。方法：患者41例，根据所用降压药（钙离子拮抗药、ACEI、ARB）将患者分为对照组、观察组A和观察组B，比较用药0，1，2，3及〉3个月时的红细胞计数（RBC）及血红蛋白（Hb）。结果：对照组患者在用药0，1，2，3及〉3个月时的RBC及Hb逐渐增加（P〈0．05）；观察组A和观察组B患者在用药0，1，2，3及〉3个月时的RBC及Hb无明显变化（P〉0．05）。结论：ARB和ACEI都可影响EPO纠正贫血的疗效，但ARB在疗效是否略优于ACEI类药物，尚无确定结论。     

Activity of the enzymes of the antioxidative system in cadmium-treated Oxya chinensis (Orthoptera Acridoidae)

One purpose in this research was to determine the toxic effects of Cd on antioxidant enzymes of Oxya chinensis (Orthoptera: Acridoidae). Changes in the activities of the antioxidant enzymes superoxide dismutase (SOD), catalase (CAT), and guaiacol peroxidase (GPx) were measured in O. chinensis insects injected with Cd²⁺. Fifth-nymphs of O. chinensis insects were injected with Cd²⁺ at different concentrations (0, 0.55 × 10⁻⁴, 1.10 × 10⁻⁴, 1.65 × 10⁻⁴, 2.20 × 10⁻⁴, and 2.75 × 10⁻⁴ g g⁻¹). An increase in SOD activity in O. chinensis was observed at 1.10 × 10⁻⁴ to 2.75 × 10⁻⁴ g g⁻¹ Cd²⁺. The SOD activity was lower at 2.20 × 10⁻⁴and 2.75 × 10⁻⁴ g g⁻¹ than that at 1.10 × 10⁻⁴ and 1.65 × 10⁻⁴ g g⁻¹. It appears that SOD had a positive protective effect at low Cd²⁺ concentrations, and that this effect disappeared at high Cd²⁺ concentrations. CAT activity was accelerated to varying degrees at 1.10 × 10⁻⁴ to 2.75 × 10⁻⁴ g g⁻¹ for males and at 1.10 × 10⁻⁴, 2.20 × 10⁻⁴, and 2.75 × 10⁻⁴g g⁻¹ for females. CAT showed a strong detoxification effect with all treatments. GPx activity decreased with increasing Cd²⁺ concentration with all treatments for males and at 2.20 × 10⁻⁴ and 2.65 × 10⁻⁴g g⁻¹ for females. We showed that GPx activity had a weak detoxification function with all treatments for males and at high Cd²⁺ for females. Thus, CAT had a strong detoxification effect, whereas SOD had a medium and GPx had a weak detoxification effect. Among the three enzymes, CAT played an important role in the damaging mechanisms of reactive oxygen species in O. chinensis insects. Alterations of the antioxidant enzyme level under environmental stresses are suggested as indicators of biotic and abiotic stress.