几种固相萃取新技术近十年的研究进展（英文）

固相萃取技术是近年来发展较快并得到广泛应用的一种样品前处理方法 （分离、纯化、富集）, 具有节省时间、溶剂消耗少, 富集倍数高, 准确度高等优点。随着科学技术的不断发展及研究的不断深入, 多种优于传统固相萃取技术的新型固相萃取新技术如分子印迹固相萃取、磁性固相萃取、固相微萃取等不断出现并广泛应用到食品、药品、生物及环境监测等领域。本文对几种固相萃取新技术的基本原理、方法及近十年来在不同研究领域的研究应用进行综述。     

固相萃取技术及其在体内药物分析中的应用

目的：了解固相萃取技术进展及应用情况。方法：从萃取机制、方法建立和萃取装置等对固相萃取技术进行综述，并对近年来该技术在体内药物分析方面的应用作了介绍。结果和结论：固相萃取技术萃取回收率高、易于自动化，能有效去除样品中的杂质等，适于生物样品的预处理。     

固相萃取技术在中药分析中的应用

目的 为复杂中成药有效成分分析和固相萃取技术的应用提供思路.方法 从7个方面总结了固相萃取技术在复杂中成药有效成分分析中的应用实例及实践经验.结果与结论 固相萃取技术可在复杂中药分析的前处理方面发挥越来越大的作用.     

生物样品预处理技术及应用进展

分析生物样品中的药物,因其复杂多样性而对样品的预处理技术提出了更高的要求。本文综述了相关文献报道的几种较新型生物样品预处理技术:固相萃取技术、超临界流体萃取技术、固相微萃取技术及其在生物样品分析中的应用。     

固相萃取技术及其在体内药物分析中的应用

目的了解固相萃取技术的新进展及其在体内药物分析中的应用情况。方法介绍固相萃取基本原理、填料种类和自动化操作等,并对该技术在体内药物分析中的应用进行综述。结果与结论固相萃取技术萃取回收率高、易于自动化,能有效去处样品中的杂质,适于体内药物分析中生物样品的预处理。     

分子印迹聚合物的制备及其在临床药物分析中的应用进展

本文综述了近年来以分子印迹材料为基础的药物分析新方法及其在临床样本（血浆、尿液）中的应用，详细评述了基于分子印迹技术的固相萃取、固相微萃取、磁性固相萃取、传感器和酶联免疫分析等最新进展，为我国临床药物分析新方法研究提供参考。     

固相萃取技术在中成药及保健食品非法添加检测中的应用进展

通过总结固相萃取技术原理及特点，查阅应用固相萃取技术检测中成药及保健食品中非法添加成分的文献，对同相萃取技术应用于中成药及保健食品非法添加成分检测的可行性进行分析，对其应用前景进行展望。     

固相微萃取技术及其在药物分析中的应用

固相微萃取（SPME）是基于固相萃取（SPE）技术发展起来的,为一种集萃取、浓缩、解吸、进样等功能于一体的样品前处理方法。本文简要介绍了SPME技术的历史、工作原理、萃取装置及萃取方法等方面内容,并结合萃取方法,介绍了SPME技术在溶剂残留、体内药物分析、中药分析等药物分析相关领域中的应用。     

固相微萃取技术及其在药物分析领域中的应用

固相微萃取是基于萃取涂层与样品之间的吸附／吸收-解吸平衡而建立起来的集进样、萃取、浓缩功能于一体的新技术。本文评述了固相微萃取技术的装置、工作原理、操作方法、影响因素及优缺点，介绍了SPME技术在药物分析中的应用近况，并且展望了这一技术的应用前景。     

自制固相萃取小柱用于中药提取液除杂的效能评价

目的评价固相萃取方法用于中药提取液除杂的效能。方法采用高效液相色谱法对中药材水煎液固相萃取前后除杂效果进行评价。结果固相萃取技术可以用于中药提取液的净化处理。结论固相萃取技术对中药提取液的有效成分保留较少,且净化效果较好,适合小批量中药口服液的纯净处理。     

An evaluation of sample preparation techniques for the GC/MS analysis of urinary mercapturic acid conjugates.

Recovery rates of four different techniques for the preparation of human urine samples spiked with N-acetyl-S-benzyl-L-cysteine (BMA) were compared at three different spiking levels. At concentrations of 1,000 ppm and 1 ppm in the urine, recoveries of BMA were greatest (80-96%) using an ion pair phase transfer technique and a C18 solid-phase extraction (C18) technique while an acidic ethyl acetate extraction method yielded 67-69% recoveries and a quaternary amine solid-phase extraction technique showed poor recoveries (5-7%). At 10 ppb, quantitative recovery could only be determined for the C18 technique due to interferences from samples prepared using the other three techniques. The results indicate that the C18 sample preparation technique followed by GC/MS analysis using stable isotopically labeled internal standards provides a rapid and accurate method for quantitation of mercapturic acids at low-ppb levels in the urine.     

Comparative study of extraction methods for the GC and GC-MS screening of urine for beta-blocker abuse

Comparison is made between conventional liquid—liquid extraction and solid-phase extraction techniques using Extrelut-1, Extrelut-3 and C18-RP cartridges respectively for the screening of several β-blockers in urine. Generally, using GC with nitrogen specific detection as the screening technique, liquid—liquid extraction and Extrelut-1 solid-phase extraction seem to be the methods of choice. However, when the screening and confirmation are performed by GC-MS, solid phase extractions with C18 or Extrelut-1 are valuable alternatives to conventional extraction. Using the different extraction techniques, detection limits and time periods during which the drugs are detectable in urine after oral administration of subtherapeutic amounts of several β-blockers are determined.     

Novel strategies for sample preparation in forensic toxicology

This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.     

Solid-phase extraction and gas chromatographic- mass spectrometric determination of the veterinary drug xylazine in human blood

This paper presents a method for the determination of xylazine in whole blood using solid-phase extraction and gas chromatography-mass spectrometry. This technique required only 0.5 mL of sample, and protriptyline was used as internal standard (IS). Limits of detection and quantitation (LOQ) were 2 and 10 ng/mL, respectively. The method was found to be linear between the LOQ and 3.50 microg/mL, with correlation coefficients higher than 0.9922. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The analyte was stable in the matrix for at least 18 h at room temperature and for at least three freeze/thaw cycles. Mean recovery, calculated at three concentration levels, was 87%. To the best of our knowledge, this is the first time that solid-phase extraction is used as sample preparation technique for the determination of this compound in biological media. Because of its simplicity and speed when compared to other extraction techniques, the herein described method can be successfully applied in the diagnosis of intoxications by xylazine.     

从红豆杉树皮浸膏中提取紫杉醇初分离工艺的研究

从红豆杉树皮浸膏中高效提取紫杉醇。方法;采用液－液萃取、固相萃取、硅胶柱层析、氧化铝柱层析、薄层层析五种分离方法对紫杉醇进行了初分离。结果：优化的紫杉醇初分离方案为红豆杉树皮提取物先经氧化铝柱,再上固相萃取柱进行分离提取。结论：该工艺分离所得紫杉醇浓度可达４０％以上,紫杉醇的回收率超过１０％。     

Performance evaluation of thermal desorption system (TDS) for detection of basic drugs in forensic samples by GC-MS

Stir bar sorptive extraction is an innovative sample extraction technique that can be used to process blood, urine, and tissue samples for routine drug screening in the forensic toxicology laboratory. The Gerstel Twister desorption unit (TDU) system is a multifunctional desorption unit capable of determining the presence of analytes from liquid samples after extraction using the Twister stir bar. The TDU desorption system was evaluated for use in combination with gas chromatography-mass spectrometry (GC-MS) for determining the presence of basic drugs in forensic samples. Human blood fortified with known quantities of drugs was used to evaluate sample diluents, extraction time, injection parameters and recovery. Case specimens containing drugs typically encountered in forensic samples were evaluated using the desorption method and compared with a liquid-liquid extraction method followed by GC-MS analysis. This evaluation demonstrated that the TDU desorptive method worked equally as well as the routine extraction method for the detection of basic drugs in screening forensic samples. In addition, the described technique avoids the use of extraction solvents and the subsequent centrifugation, transfer, and concentration steps required of liquid-liquid and solid-phase extraction methods.     

固相萃取—高效液相色谱法测定氯雷他定的血药浓度(英文)

目的建立固相萃取-高效液相色谱法测定氯雷他定血药浓度的方法。方法采用ODS-C18小柱处理样品,Zorbax SB-C18硅烷键合硅胶柱(4.6mm×250mm,5um),流动相:50mmol.L-1磷酸二氢铵缓冲液(磷酸调PH4.0)-乙腈(62∶38),流速:1.2mL.m in-1,检测波长:275nm。结果线性范围1~100 ng.mL-1(r=0.999 6),回收率在82.63%~92.41%,日内、日间RSD<10%,最低定量浓度为1ng.mL-1。结论该法简便、快速、准确,适用于氯雷他定药代动力血和生物等效性研究。     

Selective solid-phase extraction of mexiletine from human serum prior to its GLC analysis

A rapid and sensitive method for the GLC determination of mexiletine in human serum is described. The liquid-liquid extraction was replaced by the solid-phase extraction procedure for sample preparation using Separcol SI C 18 cartridges. The two-step elution of the cartridges after serum application was used-first with 50% acetonitrile in water for eluting endogenous compounds from serum, then with methanol to displace purified mexiletine. The recovery by this procedure was 83.6%. This selective solid-phase extraction offers an acceptable alternative to liquid extraction, and in combination with GLC-FID analysis is suitable for clinical pharmacokinetic studies of mexiletine.     

Bioequivalence assessment of diltiazem preparations by means of discriminant analysis of data from solid-phase extraction and liquid chromatography

A solid-phase extraction technique for sample clean-up coupled with a new LC procedure is reported for the assay of diltiazem in plasma. The use of disposable cartridges provides selective extraction and easy automation. A new LC system based on LiChrospher RP 60 Select B columns is described. For routine analysis, the procedure provides a rapid simultaneous clean-up of several samples prior to chromatography and reproducible recoveries over a concentration range of 10-800 ng. The procedure was used to analyse the plasma samples from a bioequivalence study of three commercial diltiazem preparations. The pharmacokinetic parameters in 12 healthy male volunteers were determined and the assessment of bioequivalence was conducted by discriminant analysis.