色谱新技术在体内药物分析中的应用

综述了国内外用于体内药物分析的一些新兴色谱技术,如色谱-固相微萃取联用法、色谱-质谱联用法、色谱-色谱联用法、超临界流体色谱法、毛细管电泳法、分子生物色谱法、手性色谱法等的具体应用进展;展望了色谱技术在体内药物分析应用中的前景及其发展方向,即开发新的检测技术及借助计算机手段,以实现其连续化、自动化、联用化及智能化.     

气相色谱-质谱联用法在体内药物分析方面的应用

目的:综述气相色谱-质谱联用法在体内药物分析方面的应用.方法:查阅国内外近10年来有关文献,进行分析、归纳和综述.结果:该法在植物药、兴奋剂、特殊管理药、心血管药和非甾体抗炎药等体内药物分析中已广泛应用.结论:气相色谱-质谱联用法在体内药物分析方面具有广阔的前景.     

丙泊酚的体内药物浓度分析方法研究进展

目的：为准确测定丙泊酚的体内药物浓度提供参考。方法：查阅文献,对常用的几种丙泊酚的体内药物浓度分析方法进行归纳和总结。结果与结论：丙泊酚的体内药物浓度分析常用方法包括高效液相色谱法、液相色谱．质谱联用法和气相色谱．质谱联用法,每种方法都各有其利弊,且其线性范围均能满足临床需要。不同的药物浓度分析方法具有不同的灵敏度和特点,其中高效液相色谱法相对比较常用。新的更精密的分析方法还有待进一步探索。     

减肥保健食品中添加化学药物的快速检测方法研究

目的建立薄层色谱法和液相色谱-质谱联用法检测常见减肥类保健食品中添加的化学药。方法运用薄层色谱法快速初筛,液相色谱-质谱联用法定性鉴定的色谱光谱综合运用技术。结果建立的方法能够系统而快速地鉴别出添加的盐酸西布曲明、盐酸芬氟拉明、酚酞、士的宁、盐酸麻黄碱、氢氯噻嗪等化学药物成分。结论本方法准确可靠、简便易行,易于推广。     

液相色谱-电喷雾离子肼质谱联用法在体内药物分析中的应用

在现代药物研发中,液相色谱-质谱联用法对药物的吸收、分布、代谢和消除分析是一种强有力的工具。电喷雾离子肼作为一种质谱检测模式,可产生MSn多级裂解碎片峰,进而获得丰富的结构信息,在体内药物分析时可利用这些碎片峰(MSn)建立一种强专属性和高灵敏度的高效液相色谱-质谱联用(HPLC-MS)方法。该文评述了高效液相色谱-电喷雾离子肼串联质谱(HPLC-ESI-MSn)方法在体内药物分析中的应用。     

中药制剂中非法掺入化学药物的研究近况

目的：近年来中药制剂中非法添加功效相似的化学药物时有发生，目前从中鉴别检查化学药物的方法主要有：薄层色谱法、高效液相色谱法、液相色谱-质谱联用法、高效毛细管电泳法、红外光谱法，这些研究为制定相应的技术检验标准提供了依据。     

雌激素及其代谢产物分析方法的研究进展

目的综述雌激素及其代谢产物的分析方法。方法查阅相关文献36篇,系统阐述了生物样本中雌激素及其代谢产物的前处理方法,包括水解法、萃取法、衍生化方法以及其分析方法,包括免疫分析法、气相色谱-质谱联用法及液相色谱-质谱联用法。结果免疫分析法具有高灵敏度、高通量等特点,但是容易出现交叉反应,准确性欠佳;气相色谱-质谱联用法在生物样品的雌激素类成分分析中应用广泛,但其预处理过程较为繁琐;液相色谱-质谱联用法具有强专属性、高灵敏度、高准确性和强重复性等特点,特别适用于体系组分复杂、干扰严重的样品中痕量组分的分析测定。结论液相色谱-质谱联用技术为临床上检测内源标志性雌激素类化合物提供了一种简便、快速、可靠的定性、定量分析方法,对乳腺癌的预测、预防和治疗有重大意义。     

中成药与保健品中非法添加化学药物的检测方法

（1. ［摘要］在中成药及保健品等制剂中非法添加化学药物是当前不法分子常用的制假手段之一,目前主要检测方法有化学反应法、薄层色谱法、高效液相色谱法、液相色谱 质谱联用法、高效毛细管电泳法、红外光谱法等。这些方法的应用为相关部门的打假工作提供了强有力的技术保障。作者就近几年来有关中成药及保健品中非法添加化学药物的检测方法作了综述。     

中药保健品中非法添加磷酸二酯酶-5抑制剂检测方法的研究进展

本文综述了中药保健品中非法添加磷酸二酯酶-5（PDE-5）抑制剂的检测方法。目前,快速检测一般采用红外光谱法、近红外光谱法、薄层色谱与拉曼光谱联用法等;确证检测采用高效液相色谱法,液相色谱-质谱联用法等;在结构鉴别和确证上采用核磁共振法、气相色谱-质谱联用法等补充检测;还有一些X射线衍射、酶联免疫吸附等高效检测方法,为药品监督管理部门进行该类中药保健品掺杂的检测提供相关的技术方法,保障人民食品药品合理、安全的使用。     

色谱新技术在体内药物分析中的应用进展（上）

现代色谱法已成为体内药物分析学中复杂体系组分分离和分析的强有力工具。二十一世纪,体内药物分析学在方法和技术上迅速发展,如联用技术,高通量技术,微量研究,微型化技术等,由色谱．光谱联用阶段向着在线预处理-色谱-光谱．生物技术-电子计算机等多元联用技术的方向迈进。这些先进的分析技术的改进,已经逐步应用于药物的研发与临床检测,为药物在体内乃至细胞水平的灵敏、准确、快速检测提供了可能。     

Confirmation of EMIT cannabinoid assay results by bonded phase adsorption with thin layer chromatography

Clinical urine specimens were screened for the presence of cannabinoids using the EMIT Cannabinoid Assay. Aliquots of these samples were also analyzed for 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid (THCA), the major cannabis metabolite in urine, by a technique which combines bonded phase adsorption (BPA) and thin layer chromatography (TLC). A 100% agreement between EMIT and BPA-TLC results was observed when at least 20 mL of urine was assayed by BPA-TLC. Bonded phase adsorption coupled with thin layer chromatography appears to be a suitable technique for the confirmation of positive EMIT Cannabinoid Assay results.     

Determination of SCN--in vegetables by gas chromatography in relation to endemic goiter

The quantity of thiocyanate ion in vegetables has been determined due to its relationship with endemic goiter. The technique is based on the use of gas chromatography with electron capture detection (ECD), which provides good sensitivities.     

Identification of the anabolic steroid 6β‐chlorotestosterone in a dietary supplement

Capsules that were labeled to be performance‐enhancing dietary supplements obtained during an investigation were found to contain an unrecognized steroid‐like substance. This compound was isolated by liquid chromatography (LC) fraction collection and characterized using several qualitative analytical techniques, including ultraviolet (UV) spectroscopy, gas chromatography–mass spectrometry (GC–MS), liquid chromatography‐high resolution accurate mass‐mass spectrometry (LC–HRAM–MS), as well as ¹H, ¹³C, and two‐dimensional nuclear magnetic resonance (NMR) spectrometry. This multi‐technique analytical approach was used to identify the designer steroid as 6β‐chloro‐4‐androsten‐17β‐ol‐3‐one (6β‐chlorotestosterone), an analog of testosterone about which little has been published.     

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.     

Planar chromatography: current status and future perspectives in pharmaceutical analysis (short review)--II. Special techniques and future perspectives in planar chromatography.

The state of the art of various special analytical planar chromatographic methods is summarized especially for forced-flow planar chromatography (FFPC), overpressured-layer chromatography (OPLC) and rotation planar chromatography (RPC) as well as for the automated multiple development (AMD) technique. The connection between analytical planar and column liquid chromatographic methods and the identification of separated compounds with chromatographic and spectroscopic data are summarized. Some aspects of future perspectives, such as parallel connected multi-layer FFPC and long distance OPLC (LD-OPLC) are given. A combination of OPLC with the AMD method is predicted as the method of the future. Strategies using FFPC techniques are suggested in the form of a flow chart.     

Quantitative analysis of pharmacokinetic study samples by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS).

The basis of all pharmacokinetic evaluations are powerful assays to quantify drugs and/or metabolites in biological matrices using modern sensitive instrumental analytical techniques, such as capillary gas chromatography and high-performance liquid chromatography (HPLC). Being both specific and universal, mass spectrometry (MS) is an ideal chromatographic detector. Due to recent exciting achievements in the interfacing of liquid chromatography (LC) and MS, LC-MS, like the successfully preceding hyphenated technique gas chromatography-mass spectrometry (GC-MS), has now become a valuable technique in the analyst's toolbox. The key features of LC-MS are explained and four examples demonstrating its potential for highly specific and sensitive routine drug assays with the option of high sample throughput in pharmacokinetic investigations are presented.     

Evaluation of a new Seralyzer assay for carbamazepine

The performance of a new dry-phase, strip immunoassay technique for the analysis of serum carbamazepine concentrations (Seralyzer), was compared to a standard high performance liquid chromatography (HPLC) method. One hundred blood samples were collected from 87 patients and analysed using both techniques. There was no significant difference between the concentrations measured by either technique, and the results were highly correlated (r = 0.97). The Seralyzer is a rapid and accurate method for use in carbamazepine therapeutic drug monitoring.     

Tandem mass spectrometry (LC-MS-MS): a predominant role in bioassays for pharmacokinetic studies

Plasma concentrations of drugs and drug metabolites in bioavailability studies are routinely bioassayed with high performance liquid chromatography (HPLC), gas chromatography (GC), and liquid chromatography coupled with tandem mass spectrometry (LC-MS-MS) methods. In the 1980s and 1990s, HPLC had achieved a relevant role compared to GC and other techniques in pharmacokinetic bioassays. However, in the last few years the LC-MS-MS technique, known as tandem mass spectrometry, has attained a predominant role over all other techniques. This is because it requires a less amount of matrix, possesses better specificity and sensitivity, and requires a shorter operating time. In the experience of the authors, LC-MS-MS in fact requires on average 3-4 fold shorter time to complete a bioequivalence study when performed by one operator than does HPLC. The higher cost of the apparatus and technical assistance of LC-MS-MS are fully compensated by the shorter operating time. Part or most of the HPLC apparatuses have been or are being replaced by LC-MS-MS systems in laboratories operating in clinical and pre-clinical pharmacokinetics and, to a large extent, in those involved in assessing permeability in screening procedures of new chemical entities. This paper analyses the growing development of the LC-MS-MS technique and compares four couples of methods validated with HPLC or GC versus LC-MS-MS, giving analytical details of the two approaches.     

用胶束色谱法研究非甾体抗炎药的疏水性

本文使用胶束色谱法研究了某些非甾体抗炎药的疏水性。检查了胶束色谱保留值与文献logPow的相关性。观察了表面活性剂SDS浓度的影响。对于胶束洗脱剂,logK'与logPow的相关好于k与logPow.与logk'w((甲醇—水为洗脱剂得到的外推容量因子)相比,logk'与logPow的相关性较好。logKMw(胶束—水结合常数)或logK'o(胶束浓度为零时的保留因子)与logPow也存在着线性相关。结果表明在药物定量构效关系的研究中使用胶束色谱进行药物疏水性的定量测定是很有希望的。