Sirén H, Saarinen M, Hainari S, Lukkari P, Riekkola M L
Department of Chemistry, University of Helsinki, Finland.
J Chromatogr. 1993 Feb 19;632(1-2):215-27. doi: 10.1016/0021-9673(93)80047-c.
A simultaneous screening method for atenolol, acebutolol, metoprolol, oxprenolol, alprenolol and propranolol by ion-pair chromatography with a column-switching technique was developed. The serum samples were purified using either liquid-liquid extraction or solid-phase extraction methods. The pretreatment of the samples consisted of hydrolysis and protein precipitation. The drug separation was on either octadecylsilica or polymer-based alkyl column material. Binary eluent mixtures containing methanol and a buffer solution with a quaternary ammonium salt as an ion-pair former were used. Detection of the compounds in liquid chromatographic analysis was based on ultraviolet spectra. The effects of methanol, two buffers and the ion-pair former on the retention of the compounds were studied. The determination limits ranged from nanograms to micrograms in the ion-pair chromatographic method, depending on the drug studied. Identification was based on the mass spectra or, if necessary, on selected-ion monitoring spectra of either the methylated or the acetylated compounds obtained by means of gas chromatography-electron impact or negative chemical ionization mass spectrometry. The detection limits for the identified compounds were in the picogram range. The matrix effect was strong, and this resulted in determination limits in the nanogram range with the scan method.
建立了一种采用柱切换技术的离子对色谱法同时筛选阿替洛尔、醋丁洛尔、美托洛尔、氧烯洛尔、阿普洛尔和普萘洛尔的方法。血清样品采用液-液萃取或固相萃取方法进行纯化。样品的预处理包括水解和蛋白质沉淀。药物分离采用十八烷基硅胶或聚合物基烷基柱材料。使用含有甲醇和以季铵盐作为离子对试剂的缓冲溶液的二元洗脱剂混合物。液相色谱分析中化合物的检测基于紫外光谱。研究了甲醇、两种缓冲液和离子对试剂对化合物保留的影响。在离子对色谱法中，根据所研究的药物，测定限范围为纳克至微克。鉴定基于质谱，必要时基于通过气相色谱-电子轰击或负化学电离质谱获得的甲基化或乙酰化化合物的选择离子监测光谱。已鉴定化合物的检测限在皮克范围内。基质效应很强，这导致扫描法的测定限在纳克范围内。
