Degel F
Institut für Klinische Chemie und Laboratoriumsmedizin, Klinikum Nürnberg Nord, Germany.
Clin Biochem. 1996 Dec;29(6):529-40. doi: 10.1016/s0009-9120(96)00096-3.
Newly presented solid-phase extraction methods (Solid Phase Disc Extraction, SPEC-Plus, Multi-Modal, and Solid Phase Micro Extraction, SPME have been checked with respect to their applicability to clinical toxicological analysis. In comparison with conventional liquid/liquid-extraction and a common mixed-phase column technology, their use in general screening and selective extraction methodology is discussed.
Recovery studies were performed with urine-based samples including model substances, as well as drugs and metabolites from native urine samples. Chromatographic performance of the resulting extracts is presented in some examples.
Liquid/liquid extraction, common mixed-phase column technique and the new SPEC-Plus, Multi-Modal disc extraction method gave the best recoveries with respect to broad-spectrum general screening. The purity of the concentrates was somewhat different, however. Solid-phase C18 and Solid-Phase Micro Extraction methodologies are better suited for selective drug extraction. In SPEC Disc or SPME extraction, the use of solvents is greatly reduced or omitted. Recovery of some volatile substances is enhanced. SPEC discs can be inserted directly into TLC chromatographic plates, SPME fibers into GC injection ports.
The new solid-phase extraction technologies offer advantages in different respects: The mixed-phase disc extraction SPEC 1 Plus AR/MP3 Multi-Modal delivers promising results with respect to broad-spectrum general screening. Solvent consumption is low, throughput times are short, the extracts are clean, and recovery rates are good, comparable, or even higher than with common mixed-phase column techniques. The new SPME extraction method shows benefits in dedicated, selective extraction procedures (e.g., analysis of volatile substances such as amphetamines). Sampling is solvent-free, the handling is easy, and the yields of extraction are good, but only for selected substances. Broad-spectrum general screening still remains problematic with this technique. Further examinations have to be carried out including a larger number of drugs of toxicological relevance. Headspace sampling by SPME offers a good alternative to conventional mechanized sampling in the analysis of volatile substances in biological samples, omitting the need for expensive instrumentation.
对新出现的固相萃取方法(固相圆盘萃取法、SPEC-Plus、多模式萃取法以及固相微萃取法,即SPME)在临床毒理学分析中的适用性进行了检验。与传统液/液萃取法和常见的混合相柱技术相比,讨论了它们在一般筛查和选择性萃取方法中的应用。
使用包括模型物质以及来自天然尿液样本的药物和代谢物的尿液样本进行回收率研究。在一些示例中展示了所得提取物的色谱性能。
就广谱一般筛查而言,液/液萃取法、常见混合相柱技术以及新的SPEC-Plus多模式圆盘萃取法回收率最佳。然而,浓缩物的纯度有所不同。固相C18和固相微萃取方法更适合选择性药物萃取。在SPEC圆盘或SPME萃取中,溶剂的使用量大幅减少或被省去。一些挥发性物质的回收率提高。SPEC圆盘可直接插入TLC色谱板,SPME纤维可插入GC进样口。
新的固相萃取技术在不同方面具有优势:混合相圆盘萃取SPEC 1 Plus AR/MP3多模式在广谱一般筛查方面给出了有前景的结果。溶剂消耗低,通量时间短,提取物干净,回收率良好,与常见混合相柱技术相当,甚至更高。新的SPME萃取方法在专门的选择性萃取程序(例如苯丙胺等挥发性物质的分析)中显示出优势。采样无需溶剂,操作简便,萃取产率良好,但仅适用于特定物质。该技术在广谱一般筛查方面仍然存在问题。必须进行进一步的检验,包括更多具有毒理学相关性的药物。在生物样本中挥发性物质的分析中,SPME顶空采样为传统机械化采样提供了一个很好的替代方法,无需昂贵的仪器设备。