液-质联用中大气压电离接口技术及其在药物分析中的应用

目的：介绍液相色谱-质谱联用技术（LC-MS）在药物分析中的应用。方法：通过介绍液相色谱-质谱技术原理，引入大气压电离接口技术，并综述了在药物分析中的应用。结果：液相色谱-质谱技术对药物的杂质检查与降解产物、药动学、药物代谢产物的分析和鉴定、生物大分子以及药物开发得到了广泛应用。结论：大气压电离接口技术，扩大了液相色谱-质谱联用技术的应用范围，促进了药物分析学科的发展。     

液相色谱-质谱/串联质谱联用技术及其在药物分析中的应用

液相色谱-质谱联用技术结合了色谱、质谱两者的优点，将色谱的高分离性能和质谱的高鉴别特点相结合，组成了较完美的现代分析技术。本文介绍近年来液相色谱-质谱接口技术的研究进展及液相色谱-质谱／串联质谱联用技术等在药物分析中的应用，包括药物研究的分离与鉴定，药物动力学研究的体内浓度分布、代谢物分析等，展示了它的发展前景。随着液相色谱-质谱接口技术的不断完善，液质联用技术将在药物分析中占据越来越重要的地位。     

HPLC-DAD-MS鉴定注射用雷贝拉唑钠杂质及其特征谱研究

目的利用高效液相色谱-二极管阵列检测器-质谱联用方法对注射用雷贝拉唑钠中杂质成分进行分析和结构推断。方法采用CenturySIL C18 BDS色谱柱(250 mm×4.6 mm,5μm),以磷酸盐缓冲液(磷酸氢二钠1.119 g和磷酸二氢钠0.179 g水溶液)-乙腈(体积比60∶40)为流动相,检测波长286 nm,流速1.0 mL·min-1,柱温(35±0.15)℃,进样量10μL,检测雷贝拉唑钠及其杂质;通过DAD检测器和质谱,获得在线紫外光谱图和质谱数据。结果通过在线紫外光谱图和质谱结果推断出可能含有的杂质结构,并测定了主要杂质含量限度。结论高效液相色谱-二极管阵列检测器-质谱联用技术可用于注射用雷贝拉唑钠中杂质的定性推断和定量测定。     

液相色谱——质谱联用技术及其在天然药物分析中的应用

目的　介绍近年来液相色谱—质谱联用技术的研究进展及其在天然药物分析中的应用。方法　主要介绍液相色谱—质谱(LC -MS)接口技术中API技术的研究进展及液相色谱 -电喷雾离子化质谱(LC -ESI -MS)。液相色谱 -大气压化学离子化质谱(LC -APCI -MS)等技术在天然药物分析中的应用。结果及结论　液相色谱 -质谱在接口技术方面取得了很大进展,且随着该技术的不断完善液质联用技术在天然药物分析中占据越来越重要的地位     

微透析与液相色谱-质谱联用在药物分析中的应用

目的综述微透析与液相色谱-质谱联用技术在药物体内化学成分分析中的研究进展。方法参阅近几年国内外相关文献,对微透析与液相色谱-质谱联用技术在药物体内内源性物质及外源性物质中的应用进行归纳与总结。结果与结论微透析与液相色谱-质谱联用作为一种新型的分析技术,具有快速简便、干扰少、前处理简单等优点。此项技术在体内药物分析中得到了迅速推广和应用,特别在药代动力学研究中显示出其独特的优势,具有十分广阔的应用前景     

液相色谱与质谱联用技术在药物研究中的应用

液相色谱和质谱联用（LC—MS）技术将色谱的高分离性能和质谱的高选择性相结合,具有检测样本多样性、重复性好,是一种高效快速、高选择性、高灵敏度的新型分离分析技术,非常适合活性成分复杂、含量低的药物研究。本文综述了液相色谱与质谱联用技术近年来的发展和在药物研究中的应用,该技术已成为药物研究和质量控制的有效手段之一。     

液相色谱-质谱联用技术在药物分析中的应用

液相色谱-质谱（LC—MS）联用技术体现了色谱和质谱优势的互补,将色谱的高分离性能和质谱的鉴别力强的特点相结合,组成了较完美的现代分析技术。本文介绍近年来液-质联用技术在药物分析研究领域的应用,随着液相色谱一质谱质联用技术的不断完善、发展,必将在药物分析中占据越来越重要的地位。     

联合使用反相液相色谱,柱切换以及两性离子交换-反相亲水性相互作用混合模式色谱-质谱法分析抗生素中的杂质

建立并优化了一种二维柱切换、高效液相色谱-质谱联用（LC-MS/MS）系统,用于分析抗生素及其有关物质。在一维色谱中,采用两性离子交换-反相亲水性相互作用（ZIC-RP-HILIC）混合模式色谱柱对目标杂质进行分离,并采用液质联用技术（LC-MS/MS）进行检测。在二维色谱中,采用常规的反相LC色谱柱对供试品及其杂质进行分析。ZIC-RP-HILIC混合模式色谱系统的流动相为一种适用于LC-MS/MS的可挥发性缓冲盐,能够提高杂质的离子化效率,便于对目标杂质进行结构解析。直接采用ZIC-RP-HILIC-MS系统,对使用离子对反相色谱分离的抗生素杂质进行定性分析。ZIC-RP-HILIC混合模式色谱与反相LC色谱系统之间的正交性,进一步保证了杂质检测的全面性。此方法的优势体现在对青霉素V钾,苯唑青霉素钠、头孢曲松钠的杂质分析中。另外,该方法便于进行抗生素的杂质谱分析,并可用于其它药物的杂质分析。     

色谱联用技术在中药研究领域的应用

中药现代化离不开现代、高效的分离、分析技术。现代分析技术的发展，尤其是色谱联用技术的出现加快了中药研发的步伐。该技术具有所需样品量少、速度快等特点，且可得到更多信息。目前，正处于快速发展阶段并广泛应用的色谱联用技术包括气相色谱-质谱联用（GC—MS）、液相色谱质谱联用（LC—MS）、高效液相-核磁共振仪联用（HPLCNMR）、毛细管电泳-核磁共振仪联用（CE—NMR）、液相色谱-质谱／质谱联用（LC一／MS／MS）、液相色谱-核磁-质谱联用（LC—NMR—MS）、毛细管电泳-质谱联用（CEMS）等，本就其在中药研究领域的应用作一简要综述。     

液-质联用在体内药物分析中的应用

目的:综述液相色谱-串联质谱联用在体内药物分析中的应用,为进一步扩大应用提供参考。方法:检索国内2008-2009年相关文献,进行分析、整理和归纳。结果:液相色谱-串联质谱联用集液相色谱的高分离效能与质谱的高鉴定性能于一体,对研究对象有足够的灵敏度、选择性,分析快速且方便,在药学研究方面的应用日益广泛。结论:液相色谱-串联质谱联用是目前最重要的分离分析方法之一,将在未来几年不断发展且在体内药物分析中发挥越来越重要的作用。     

Chromatography-mass spectrometry methods for the quantitation of statins in biological samples

The 3-hydroxy-3-methyl glutaryl coenzyme A (HMG-CoA) reductase inhibitors, more commonly known as 'statins', are a novel class of drugs widely used for the treatment of hypercholesterolaemia in patients with established cardiovascular disease as well as those at high risk of developing atherosclerosis. Published chromatographic-mass spectrometric methods for the quantification of presently available seven statins, atorvastatin, simvastatin, lovastatin, pravastatin, fluvastatin, rosuvastatin and pitavastatin are reviewed. High performance liquid chromatography (HPLC) in combination with tandem mass spectrometry (MS/MS) is the analytical technique of choice for the quantification of statins in biological samples. This review envisages that most of the methods used for quantification of statins are in plasma and they are suitable for therapeutic drug monitoring of these drugs.     

液质联用技术在环烯醚萜苷类化合物研究中的应用

液质联用技术将色谱的高分离性能和质谱强大的结构鉴别功能相结合,是较完善的现代分析技术,已广泛应用于药物定量分析、结构鉴定和代谢转化等研究。本文对液质联用技术在环烯醚萜苷类化合物定性和定量分析两方面的应用进行简要综述。     

牡丹皮化学成分的液相色谱-飞行时间串联质谱分析

目的分析牡丹皮中的化学成分。方法应用优化的高效液相色谱-质谱联用方法对牡丹皮供试品进行分析。结果较好地分离了单萜苷、鞣质和酚酮类等38种化学成分。在负离子检测模式下，由电喷雾质谱得到各成分的准分子离子峰，再根据串联飞行时间质谱获得进一步的结构信息，推测出其中38种主要成分的可能结构。并对牡丹皮中主要化学成分的质谱裂解规律进行了分析。结论本方法能快速检测牡丹皮的化学成分。     

Identification and quantitation of sodium-thyroxine and its degradation products by LC using electrochemical and MS detection

High performance liquid chromatography (HPLC) was used in combination with an amperometric and mass spectrometric detection to elucidate and quantitate the degradation products and contaminants of the photo-sensitive Na-thyroxine. Using HPLC with amperometric detection, seven decomposition compounds were separated. These products, which occur mostly as contaminants, were then identified by a developed liquid chromatography-mass spectrometry technique. The same HPLC method was also employed to analyze Na-thyroxine and its degradation products in three commercially available brands of Na-thyroxine tablets.     

Rapid and Simple Determination of Homovanillic Acid in Plasma Using High Performance Liquid Chromatography with Electrochemical Detection

Abstract: A rapid, yet highly reliable, procedure for determination of homovanillic acid (HVA) in plasma is described. After precipitation of proteins with perchloric acid, separation of sample components is directly achieved with high performance liquid chromatography on a reversed-phase column (C8), followed by quantitation based on electrochemical detection. The sensitivity of this method is 0.5 pmol/injection. Detector response is linear from the limit of detection to at least 0.5 nmol/injection. The intra-assay coefficient of variation is 2.2% in the concentration range of 50–150 pmol/ml plasma. The inter-assay coefficient of variation is 6.3%, based on determinations on 30 working days. A comparison of the present method and a specific gas chromatographic-mass spectrometric assay showed good agreement between the two procedures. One chromatographic run requires less than 16 min. for plasma and 10 min. for a standard.     

Control and analysis of hydrazine, hydrazides and hydrazones--genotoxic impurities in active pharmaceutical ingredients (APIs) and drug products

This is the latest of a series of reviews focused on the analysis of genotoxic impurities. This review summarises the analytical approaches reported in the literature relating to hydrazine, hydrazines, hydrazides and hydrazones. It is intended to provide guidance for analysts needing to develop procedures to control such impurities, particularly where this is due to concerns relating to their potential genotoxicity. Of particular note is the wide variety of techniques employed, both chromatographic and spectroscopic, with most involving derivatisation. Such a wide variety of options allow the analyst a real choice in terms of selecting the most appropriate technique specific to their requirements. Several generic methodologies, covering the three main analytical approaches; i.e. HPLC (high performance liquid chromatography), GC (gas chromatography) and IC (ion chromatography), are also described.     

A high‐throughput and broad‐spectrum screening method for analysing over 120 drugs in horse urine using liquid chromatography–high‐resolution mass spectrometry

A high‐throughput method has been developed for the doping control analysis of 124 drug targets, processing up to 154 horse urine samples in as short as 4.5 h, from the time the samples arrive at the laboratory to the reporting deadline of 30 min before the first race, including sample receipt and registration, preparation and instrument analysis and data vetting time. Sample preparation involves a brief enzyme hydrolysis step (30 min) to detect both free and glucuronide‐conjugated drug targets. This is followed by extraction using solid‐supported liquid extraction (SLE) and analysis using liquid chromatography–high‐resolution mass spectrometry (LC–HRMS). The entire set‐up comprised of four sets of Biotage Extrahera automation systems for conducting SLE and five to six sets of Orbitrap for instrumental screening using LC–HRMS. Suspicious samples flagged were subject to confirmatory analyses using liquid chromatography–triple quadrupole mass spectrometry. The method comprises 124 drug targets from a spectrum of 41 drug classes covering acidic, basic and neutral drugs. More than 85% of the targets had limits of detection at or below 5 ng/mL in horse urine, with the lowest at 0.02 ng/mL. The method was validated for qualitative identification, including specificity, sensitivity, extraction recovery and precision. Method applicability was demonstrated by the successful detection of different drugs, namely (a) butorphanol, (b) dexamethasone, (c) diclofenac, (d) flunixin and (e) phenylbutazone, in post‐race or out‐of‐competition urine samples collected from racehorses. This method was developed for pre‐race urine testing in Hong Kong; however, it is also suitable for testing post‐race or out‐of‐competition urine samples, especially when a quick total analysis time is desired.     

制备型高效液相色谱法在药物杂质研究中的应用

制备型高效液相色谱法是一种使用高压、大流量液体输送系统在高分辨率、大内径、高载量分离柱上进行样品高纯度分离的液相色谱制备方法。应用该方法分离的产品在纯度、回收率、分离效率等方面远远优于传统的制备方法,因此在药物研究、生产领域得到广泛应用。介绍制备型高效液相色谱法的研究概况,特点,影响制备型高效液相色谱分离纯化的因素,以及在药物杂质研究中的实际应用,并对制备型高效液相色谱技术存在的问题与发展方向进行总结。     

棘白菌素B母核关键杂质的制备与鉴定

采用制备液相色谱技术对棘白菌素B母核粗品中的关键杂质进行分离纯化,并通过质谱和核磁共振波谱分析鉴定杂质结构。制备的2个棘白菌素B母核杂质(化合物M和N)与棘白菌素B母核具有相同的主体结构,分别为母核F位和E位氨基酸残基的去甲基产物,为阿尼芬净的杂质研究和质量控制提供了技术支持。     

高效液相色谱在药学的应用概况和最近进展

高效液相色谱法是近年来逐渐兴起的一种高效而快速的分离与分析技术,是现代分离测试的重要方法。目前,高效液相色谱法已被广泛运用于各个领域。因其选择性好、灵敏度高、可准确分析微量组成、分析痕量样品等特点已成为医药学分析领域发展最快捷的分析技术。随着高效液相色谱法的普及,色谱仪也得到了相应的更新与改进,色谱仪也正朝着多样化、自动化、联用技术化等方向发展。本文通过对近十几年来国内发表的具有代表性的相关文章进行分析、整理和归纳,综述了高效液相色谱技术在（中）药学、食品检测、保健品检测等研究领域中的应用和最新研究进展。