HPLC法测定健宝胶囊中淫羊藿苷含量

目的　建立健宝胶囊中淫羊藿苷的含量测定方法。方法　采用高效液相色谱法 ,色谱柱为C18(15 0mm×4.6mm) ,流动相为乙腈 0 .0 75mol·L-1磷酸溶液 (2 5∶75 ) ,流速 1.0mL·min-1,检测波长为 2 70nm。结果　淫羊藿苷进样量在 0 .0 6～ 0 .30 μm范围内 ,线性关系良好 (r=0 .9991) ,方法回收率为 98.5 0 %(n =5 ,RSD =1.2 0 %)。结论　本方法准确、简便、快速 ,适合于该药的质量分析检验。     

引阳素胶囊中淫羊藿苷的含量测定

目的建立引阳素胶囊中淫羊藿苷的高效液相色谱(HPLC)含量测定方法。方法采用HPLC法。色谱柱Li-chrospher C18(4.6 mm×250 mm,5μm),C18保护柱;流动相为乙腈-20 g/L冰醋酸水溶液(30∶70);检测波长270 nm;流速1.0 mL/min;柱温为室温;进样量10μL。样品加50%(体积分数)乙醇超声提取,浸提液过0.45μm滤膜后测定。结果淫羊藿苷线性范围为10.0-60.0 mg/L,回归方程为C=2.042×10-5A+0.554,r=0.9993,平均回收率为99.8%,RSD为0.65%。结论本法用于引阳素胶囊中淫羊藿苷的含量测定时简便快捷、准确。     

高效液相色谱法测定水溶液中芘的实验研究

建立表面活性剂与有机物共存体系中芘测定的高效液相色谱法.采用C18反向色谱柱(2.1mm×100mm,5μm),通过调节和控制流动相、柱温、流速等因素,得到芘的优化测试条件.结果表明:流动相选用乙腈-水(80:20,V/V),流速0.20mL·min-1,柱温25℃是最优测试条件.同时,对TX-100存在与不存在情况下芘的测试结果进行比较分析,使用OriginPro 8.6对实验数据进行线性拟合,并进行统计学t检验,结果表明:X-100存在与否对水溶液中芘的测定没有显著影响.     

高效液相色谱法测定早期肾移植患者麦考酚酸的血药浓度

目的 建立高效液相色谱法测定人血浆中麦考酚酸浓度的简便方法.方法 采用高效液相色谱法,色谱柱为C18柱(3.9mm×300mm),以40mmoL/L四丁基溴化铵-乙腈[55∶45(V∶V),H3PO4调pH=4]为流动相,流速0.8mL/min,紫外检测波长254nm,用甲醇沉淀蛋白法进行血样处理.结果 麦考酚酸的线性范围为0.8～51.54mg/L(r=0.9998),平均相对回收率95.5%～109.2%,提取回收率>90%,批内和批间RSD<10%.结论 本方法准确、简便,可用于麦考酚酸的血药浓度监测和生物等效性研究.     

高效液相层析法测定人体血浆组胺水平

为了快速，敏感和特异地检测人体血浆组胺水平。方法应用高效液相层析技术探索Ｈｉ定量分析的最佳工作条件，并测定２２例正常人血浆Ｈｉ水平。流动相中甲醇与ＮａＨ２ＰＯ４比例为６０／４０，ｐＨ为５．１，层析柱温度为２０－３０℃时，Ｈｉ时０．５－５ｎｍ半，含量与峰面积呈正比，于９ｍｉｎ左右出峰。     

川芎药材活性部位的高效液相色谱指纹图谱定性分析方法

目的　建立川芎药材活性部位的指纹图谱 ,为其定性鉴别提供依据。方法　川芎药材经乙醇超声提取后 ,用醋酸乙酯萃取 ,采用ODS柱为分析柱 ,以甲醇 水 冰醋酸 (30∶70∶0 .5 )为流动相 ,在 2 76nm条件下进行分析 ,建立其指纹图谱。并对 7种不同来源的川芎药材进行高效液相色谱指纹图谱定性分析比较。结果　本研究建立的分析方法的精密度、重现性较好 ,以阿魏酸峰计 ,RSD分别为 1.6 8%和 1.0 4 % ;不同川芎药材指纹图谱中主要峰群的整体图貌基本一致 ,但各成分含量的相对比值有所不同 ,不同来源的川芎药材共有峰面积的比值及共有峰面积和均有一定的差异。结论　HPLC指纹图谱分析法可简便、快速地鉴别区分不同来源的川芎药材     

人血浆中茶碱的效液相色谱测定法

茶碱是临床上常用的抗喘药,它对支气管哮喘的疗效早已被肯定,但由于即使同一剂量的茶碱,在某些人为线性代谢,而另一些人已经出现非线性代谢。所以其在人体内的代谢存在着十分明显的个体差异,又由于茶碱是有一定毒性的药物,因此,有必要对人体血浆中茶碱的浓度进行监测,而建立一准确、快速、简便的监测茶碱血药浓度的测定方法,是确定其合理给药方法的前提。本文旨在建立人血浆中茶碱的高效液相色谱测定方法,并从准确性、重复性、专一性等方面对其进行考证,说明该方法符合生物样品的分析要求,以确定合理的给药方法。     

沙棘油中α-生育酚含量的反相高效液相层析分析法

为了控制沙棘油的质量,建立了一种反相高效液相层析法(RP—HPLC)测定沙棘油中α—生育酚的含量。沙棘油样品皂化后,用乙醚提取,浓缩乙醚提取液,残渣溶解于无水乙醇中注入液相层析仪。层析条件:ZORBAX柱(4.6×150mm)甲醇作流动相(1ml/min),紫外检测波长,280nm。测定了陕西永寿产沙棘种子油和果油各3批,α—生育酚的平均含量分别为989mg/kg,1754mg/kg。方法回收率98.6%(种子油),102.2%(果油),变异系数小于5.44%。     

高效液相色谱法测定胆汁中结合胆汁酸

报道反相高效液相色谱法测定人胆汁中结合胆汁酸,样品处理手续简便,因为色谱系统使用了保护柱。回收率范围是87.01%～110.75%,检出限为0.09～0.21μg,用本方法分析胆石症患者及对照组胆汁结合胆汁酸。     

多敏灵片中咖啡因和盐酸多塞平含量的测定

目的建立高效液相色谱法,测定多敏灵片中咖啡因、盐酸多塞平的含量。方法采用高效液相色谱法,以Kromasil C18(250 mm×4.6 mm,5μm)为分析柱,流动相为甲醇-水-三乙胺(75∶25∶1),流速1 mL/min,检测波长295 nm,柱温为室温。结果咖啡因、盐酸多塞平与其他组分分离良好,且不受其他成分的干扰;咖啡因回归方程为:Y=196 604X+218 976(r=0.999 8,n=5),咖啡因在0.08~0.24μg的范围内线性关系良好;盐酸多塞平回归方程为:Y=60 158X+58 230(r=0.999 9,n=5),盐酸多塞平在0.04~0.12μg的范围内线性关系良好。方法的平均回收率分别为99.06%、96.67%,精密度(RSD)值分别为1.04%、1.13%。结论本方法操作简便、快速、准确、灵敏,适用于多敏灵片的含量测定。     

Pre-concentration and determination of amitriptyline residues in waste water by ionic liquid based immersed droplet microextraction and HPLC

This paper describes a new approach for the determination of amitriptyline in wastewater by ionic liquid based immersed droplet microextraction (IL-IDME) prior to highperformance liquid chromatography ...     

Control system for low pressure gradient mixer in high performance liquid chromatograph

A control system used in high performance liquid chromatograph(HPLC) was described.The control system adopting low pressure gradient elution was tested with different initial and end volume fractions,and four types of gradient elution curves.The experimental results verified the theoretical analyses of the applied method.This self-designed control system can achieve approving accuracy,repeatability and low cost,which has a bright outlook for domestic applications.     

Sensitive determination of 4-O-methylhonokiol in rabbit plasma by high performance liquid chromatography and application

A novel high performance liquid chromatographic method was developed for the determination of 4-O- methylhonokiol in rabbit plasma and was applied to its pharmacokinetic investigation. Plasma samples were treated by one-fold volume of methanol and acetoni     

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

Objective High performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS) methods were developed for the determination of ganciclovir and its related substances. Methods A Hypersil ODS2 column (4.6mm×250mm, 5μm) was used with a mobile phase of 0.02M potassium 1.0mL/min, and UV detector set at 254nm was used for monitoring the eluents. Results The method was simple, rapid, selective and capable of separating all related substances at trace level with a detection limit of 0.04μg/mL. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 10.2-153.0μg/mL with r=0.9998. The percentage recoveries ranged from 96.7% to 101.6%, and RSD was 1.24%-1.96% (n=5). Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir. For identification of related substances, LC/MS was used. The mainly related substances of ganciclovir active pharmaceutical ingredients (API) were determined as guanine, (1, 3-dioxolan-4-yl) methyl acetate, and diacetyl guanine.     

Study on chromatographic fingerprint of sarcandra glabra （Thunb.） by microwave-assisted extraction coupled to HPLC/DAD

Microwave-assisted extraction (MAE) was used for extraction of effective components of sarcandra glabra (Thunb.), and then chromatographic fingerprint of sarcandra glabra (Thunb.) was studied by high performance liquid chromatography/diode array detector (HPLC/DAD). The conditions of MAE were optimized by an orthogonal experiment, and then the authentication and validation of the chromatographic fingerprint were conducted. Nine peaks were identified as common peaks in the fingerprint chromatograms, and isofraxidin was considered as a reference compound and quantified. Relative standard deviations of retention time and peak area of each component were less than 3% and 8%, respectively. Similarity and difference analysis were conducted by use of PCA and relation coefficient. Twenty batches of sarcandra glabra (Thunb.) samples from two different producing areas could be classified into two different groups in the PCA model. The results showed that MAE-HPLC/DAD method was simple, efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra (Thunb.), which could provide more reliable and precise information for quality evaluation.     

Determination of enantiomeric impurity of etomidate by high performance liquid chromatography

Objective To determine enantiomeric impurity of etomidate using high performance liquid chromatography. Methods (R)-etomidate and (S)-etomidate were isopropanol-n-hexane. The flow rate of the mobile phase was 0.5mL/min. The detected wavelength was 242nm. Results (R)-etomidate and (S)-etomidate could be separated completely under these conditions. The precision of (R)-etomidate was 1.57% (n=3). The limit of detection of (R)-etomidate was 4.25ng/mL. The average percentage content of (S)-etomidate was 0.09% in the samples. Conclusion The method was repeatable and sufficiently sensitive to determine the enantiomeric impurity of etomidate. It allows the quantitation of the impurities at the 0.085% (w/w) level relative to etomidate at a concentration of the test solution of 5mg/mL.     

Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitu

An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for in