米托坦人血浆浓度的UPLC快检及治疗药物监测

建立一种超高效液相色谱-紫外法(UPLC-UV)快速测定米托坦血浆中治疗药物浓度监测(TDM)的方法。血浆样本经乙腈沉淀蛋白后,采用色谱柱为C18(2.1 mm×50 mm,1.7μm),流动相：乙腈∶水(78∶22,v/v),流量：0.3 mL·min^–1,柱温40℃,在波长为230 nm处检测,外标法定量。米托坦保留时间为1.38 min,定量限(LOQ)为0.5μg·mL^–1,线性范围为0.5～50μg·mL^–1、线性回归方程为y=6 213x+197 (r²>0.999),平均回收率均大于99%;批内精密度在1.70%～6.63%之间,准确度在–6.56%～11.08%之间;批间精密度在3.99%～8.64%之间,准确度在–0.62%～1.90%之间。该方法快速简便,准确度高,适用于临床上米托坦血浆药物浓度的监测。     

RP-HPLC法测定大鼠血清中NI221的含量

建立一种快速、准确测定大鼠血清中NI221含量的RP-HPLC分析方法。以阿魏酸为内标物,360μL血清样品经冰冻乙腈蛋白沉淀处理后,取20μL上清进样分析;色谱柱为Diamonsil C18柱（200mm×4.6mm×5μm）,流动相组成为甲醇∶0.05%的磷酸=55∶45（用氢氧化钠调节pH=2.5）,流速为1.0mL·min-1,紫外检测波长为302nm,柱温为室温。血清中NI221浓度在0.15~20μg·mL-1范围内呈线性,相关系数r=0.9996,样品加标回收率为97.36%~112.50%（n=15）,日内和日间精密度RSD均〈15%。所建立的RP-HPLC方法准确可靠,重现性好,可用于临床前药代动力学研究中NI221血药浓度的测定。     

RP-HPLC法测定大鼠血清中NI221的含量

建立一种快速、准确测定大鼠血清中NI221含量的RP-HPLC分析方法。以阿魏酸为内标物,360μL血清样品经冰冻乙腈蛋白沉淀处理后,取20μL上清进样分析;色谱柱为Diamonsil C18柱(200mm×4.6mm×5μm),流动相组成为甲醇∶0.05%的磷酸=55∶45(用氢氧化钠调节pH=2.5),流速为1.0mL·min-1,紫外检测波长为302nm,柱温为室温。血清中NI221浓度在0.15²0μg·mL-1范围内呈线性,相关系数r=0.9996,样品加标回收率为97.36%20μg·mL-1范围内呈线性,相关系数r=0.9996,样品加标回收率为97.36%¹12.50%(n=15),日内和日间精密度RSD均<15%。所建立的RP-HPLC方法准确可靠,重现性好,可用于临床前药代动力学研究中NI221血药浓度的测定。     

关于亚胺培南-西司他丁钠的测定分析

亚胺培南-西司他丁钠为新型β-内酰胺类抗生素,既有极强的厂谱抗菌活性,又有β-内酰胺酶抑制作用。采用高效液相法色谱测定亚胺培南-西司他丁钠,方法可靠、简便、准确。     

HPLC法测定消癌平糖浆中绿原酸的含量

采用高效液相色谱法对消癌平糖浆中绿原酸进行含量测定。色谱柱为Diamonsil C18柱,流动相为乙腈-0．1％磷酸溶液（12：88）,检测波长为326nm,流速为1．0mL·min^-1。绿原酸在0．055—0．550μg呈良好的线性关系,相关系数r为0．9999,此方法操作简便,结果准确、可靠,回收率为98．9％。     

扶桑花中槲皮素含量的HPLC法测定

目的建立扶桑花中槲皮紊的含量测定方法。方法采用HPLC法,色谱柱为DikmaplatisilODS柱（250rain×4．6mm,5μm）,流动相为甲醇0．5％磷酸水溶液（体积比30：70）,流速1．0mL·min-1,柱温30℃,检测波长360m。结果槲皮素进样量在0．0416～0．416μg范围内与峰面积呈良好的线性关系,平均回收率为98．95％,RSD为1．09％（n=6）。结论该方法操作简便、快速、准确,可用于扶桑花药材的质量控制。     

HPLC法测定消癌平糖浆中绿原酸的含量

采用高效液相色谱法对消癌平糖浆中绿原酸进行含量测定。色谱柱为Diamonsil C18柱,流动相为乙腈-0.1%磷酸溶液(12∶88),检测波长为326nm,流速为1.0mL.min-1。绿原酸在0.055~0.550μg呈良好的线性关系,相关系数r为0.9999,此方法操作简便,结果准确、可靠,回收率为98.9%。     

应用HPLC法测定刺五加中紫丁香苷的含量

目的:采用高效液相色谱法测定不同产地刺五加中紫丁香苷的含量。方法:采用C18柱,流动相:甲醇-水(20:80),流速:1.0ml/min,检测波长:265nm。结果:伊春产刺五加紫丁香苷含量最高;但五个产地中刺五加紫丁香苷含量均远高于2005年版《中华人民共和国药典》一部中关于刺五加紫丁香苷含量的要求。     

HPLC法测定食品中苯甲酸、山梨酸和糖精钠

本实验采用LC-5500高效液相色谱仪快速测定食品中苯甲酸、山梨酸、糖精钠的高效液相色谱法。实验以YWG-C18柱,甲醇:乙酸铵为流动相,研究其三种物质的色谱分离特性,并对食品样品的前处理方法进行探讨。经实践得到了快速、有效的分离和样品处理方法。该方法测定的三种物质浓度在0～0.100mg/ml之间呈线性关系,相关系数在0.999以上,证明该法具有方法简便,灵敏度高,选择性好,线性范围宽等优点。     

HPLC法测定A颗粒中芍药苷的含量

目的:建立A颗粒中芍药苷的含量测量方法。方法:采用HPLC法对A颗粒中的芍药苷进行了含量测定。结果:芍药苷在0.1490-1.2265mg/g范围内线性关系良好。R=0.9994平均回收率为100.9%。RSD值为1.24%(n=6)。含量限度为4.5 mg/g。结论:该法可用于A颗粒中芍药苷的含量测定。     

A simple pharmacokinetic model of alendronate developed using plasma concentration and urine excretion data from healthy men

The study of pharmacokinetics of alendronate has been hampered by difficulties in accurately and reproducibly determining their concentrations in serum and urine. Thus, pharmacokinetic characteristics of alendronate have been described in many reports based on urinary excretion data; and plasma pharmacokinetics and the simultaneous pharmacokinetic models of alendronate in plasma and urine are not available. The aims of this study were to measure alendronate concentration in plasma and excretion in urine concurrently and to develop compartmental pharmacokinetic model using urine data. In open-label, single-dose pharmacokinetic study, 10 healthy male volunteers received oral dose of alendronate (70?mg tablet). Blood and urine alendronate concentrations were determined using validated high-performance liquid chromatography method. Non-compartmental analysis was performed using WinNonlin program (Pharsight Inc., Apex, NC). A one-compartment pharmacokinetic model was applied to describe pharmacokinetics of alendronate. A peak plasma alendronate concentration of 33.10?±?14.32?ng/mL was attained after 1.00?±?0.16?h. The cumulative amount of alendronate excreted in urine and peak excretion rate were 731.28?±?654.57?μg and 314.68?±?395.43?μg/h, respectively. The model, which included first-order absorption rate for oral dosing, showed good fit to alendronate data obtained from plasma and urine. The absorption rate constant was 2.68?±?0.95?h^–1. The elimination rate constants K_urine and K_non-ur were 0.005?±?0.004?h^?1 and 0.42?±?0.08?h^?1, respectively. The pharmacokinetics of alendronate in plasma and urine of healthy men can be predicted using one-compartment model, and thus the behavior of drug in plasma can be estimated from urinary excretion data.     

高效液相色谱法测定茶皂苷的含量及其血药浓度

目的:建立了高效液相色谱法对茶皂苷含量及其血药浓度的测定.方法:色谱柱为Hypersil ODS(25mm,4.6*250mm),流动相为甲醇-水(90:10),流速为0.5ml/min,检测波长为215nm.结果:茶皂苷在0.16～1.28mg/mL的浓度范围内,茶皂苷的浓度与主峰面积具有良好的线性关系,回归方程:y...     

LC-MS/MS测定猪尿中盐酸克伦特罗不确定度的评定

建立了液相色谱-串联质谱法(LC-MS/MS)测定猪尿中盐酸克伦特罗残留量的不确定度评定数学模型,分析了影响样品测定结果的不确定度的主要来源,并计算出了各影响因素的不确定度分量.当猪尿中盐酸克伦特罗残留量的测定结果为3.6ng/mL时,其扩展不确定度为0.4ng/mL.     

LC-MS/MS法测定比格犬血浆中的阿那曲唑

用高效液相色谱-串联质谱法(LC-MS/MS)测定比格犬血浆中阿那曲唑的浓度。以苯磺酸氨氯地平为内标,加入50μL血浆,用甲基叔丁基醚萃取后取上清液以氮气吹干,用50%甲醇水溶液复溶,进样5μL,在电喷雾离子源下进行正离子检测。色谱柱为Agilent XDB C18(50mm×2.1mm×3.5μm),流动相为0.1%甲酸水-0.1%甲酸乙腈(60∶40)。阿那曲唑和内标的质荷比(m/z)分别为294.4和409,阿那曲唑和内标生成的主要碎片离子的质荷比(m/z)分别为255.3和238。阿那曲唑在0.5~500 ng·mL-1内线性良好,检出限为0.5ng·mL-1,提取回收率均大于80%,日内、日间准确度为101%~104%,日内、日间精密度分别小于7.04%和8.69%,已成功检测比格犬血浆中阿那曲唑的血药浓度。所用方法稳定、灵敏度好、分析时间短、提取回收率高,适用于比格犬血浆中阿那曲唑的血药浓度测定。     

Fatigue life determination of plasma nitrided medical grade CoCrMo alloy

In this paper, the fatigue behaviour of plasma nitrided medical grade forged CoCrMo alloy was studied. Since metallic biomaterials are used for implant applications where high and/or cyclic stresses along with corrosive effects of human body are of concern, enhancing mechanical and surface properties of implant alloys is crucial. Plasma nitriding was implemented at three different temperatures as 600, 700 and 800 °C for time intervals of 1 and 4 h. S–N curves of untreated and nitrided specimens were obtained via axial tension compression fatigue tests. It was found that plasma nitriding treatment reduces the fatigue resistance of forged CoCrMo alloy by the ratios of 7–23% depending on the surface roughness, phase structure and hardness of the modified layer which are determined by the treatment parameters.     

近红外光谱尿液分析仪的原理及实现

分析了现有尿液成分分析方法,结合光谱仪工作原理和光机电设计理论,提出一种基于近红外光谱的无试剂尿液分析仪。该分析仪采用4个LED光源固定分布在圆形转盘上,系统控制步进电机带动圆盘转动实现LED循环透射样品,高速型InGaAs光电二极管作为检测器;单片机控制软件采用C51语言编制,实现对电路各模块的功能驱动;PC上位机软件采用VC++6.0编写,实现对数据采集卡传输的数据进行存储、图形显示及尿液成分分析。     

电感耦合等离子体原子发射光谱法测定电解钴中杂质元素

金属钴试样经酸消解后,未经基体分离直接以全谱直读电感耦合等离子发射光谱仪测定其中杂质元素。确定了仪器的最佳工作条件,选择了合适的分析谱线,采用钇作为内标物质,补偿基体效应。方法测定各元素的检出限在0.0001～0.02mg.L-1范围内。方法用于样品的测定,相对标准偏差为1.5%～7.5%,回收率为94.0～104.0%,各元素的测定值与国家标准方法的测定值相符合。     

Chip-based capillary electrophoresis/mass spectrometry determination of carnitines in human urine

A chip-based capillary electrophoresis/mass spectrometry (CE/MS) system is described for the CE separation and on-line electrospray detection of carnitine and selected acylcarnitines from mixtures of analytical standards as well as extracts of fortified human urine. Chip-based CE/MS experiments in two different laboratories were carried out using a triple-quadrupole mass spectrometer and a quadrupole time-of-flight (QTOF) mass spectrometer, respectively. The glass chips used with both systems were comparably equipped with a microfabricated capillary electrophoresis (CE) channel but with different electrosprayers. The quadrupole chip-based CE/MS experiments employed a miniature coupled microsprayer, which allowed coupling of the microelectrospray process via a micro liquid junction at the exit of the CE capillary channel. Selected ion monitoring (SIM) CE/MS experiments were employed for all of the quadrupole CE/MS work. The QTOF CE/MS full-scan single MS and MS/MS experiments were carried out in another laboratory using accurate mass measurement TOF mass spectrometry techniques. The electrospray process that was employed with the QTOF system differed in that an inserted nanoelectrospray capillary needle was carefully affixed into a flat-bottomed hole that was aligned with the CE channel exit orifice. SIM CE/MS using the described quadrupole system provided acceptable ion current electropherograms from fmole levels from analytical standard solutions of carnitine and acylcarnitines that were manually injected (loaded) onto the chip. In addition, the corresponding electropherograms for human urine fortified with the target carnitine and acylcarnitines at a 10-20 microg/mL (35-124 microM) level were obtained via SIM CE/MS techniques. The measured CE separation efficiency for the SIM CE/MS electropherograms was determined to be 2860 plates (peak width at half-height method or N = 5.54(T/WO.5(2)), and carnitine and three acylcarnitines were separated in less than 48 s. In contrast, using quadrupole-TOF technologies, the same samples could be diluted by a factor of 2-4 to obtain a comparable detector response for the target compounds. In the full-scan, single mass analyzer mode (m/z 150-500), the CE separation efficiency was measured to be 2600 plates, but mass measurement accuracy was less than 5.0 ppm for the quaternary cations. In the CE/MS/MS mode, full-scan collision-induced dissociation (CID) mass spectra were obtained with a mass accuracy of < or =10 ppm for the higher mass ions and < or =27 ppm for the lower mass product ions. These results demonstrate the feasibility for on-chip CE separation and electrospray mass spectrometric detection for these important compounds in synthetic mixtures, as well as in human urine extracts.