Heinig K, Henion J
Analytical Toxicology, Cornell University, New York State College of Veterinary Medicine, Ithaca 14850, USA.
J Chromatogr B Biomed Sci Appl. 1999 Sep 24;732(2):445-58. doi: 10.1016/s0378-4347(99)00313-8.
We present fast LC-MS-MS analyses of multicomponent mixtures containing flavones, sulfonamides, benzodiazepines and tricyclic amines. Using a short microbore HPLC column with small particle size, five to eight compounds were partially resolved within 15 to 30 s. TurboIonSpray and atmospheric pressure chemical ionization interfaces were well suited to tolerate the higher eluent flow-rates of 1.2 to 2 ml/min. The methods were applied to biological sample matrices after clean-up using solid-phase or liquid-liquid extraction. Good precision and accuracy (average 8.9 and 97.7%, respectively) were achieved for the determination of tricyclic amines in human plasma. Benzodiazepines were determined in human urine with average precision of 9% and average accuracy of 95% for intra- and inter-assay. Detection limits in the low ng/ml range were obtained. An example for 240 injections per hour of demonstrated the feasibility of rapid LC-MS-MS analysis.
我们展示了对含有黄酮类化合物、磺胺类药物、苯二氮䓬类药物和三环胺的多组分混合物进行快速液相色谱-质谱联用（LC-MS-MS）分析的方法。使用短的小粒径微径高效液相色谱（HPLC）柱，在15至30秒内可部分分离出五到八种化合物。TurboIonSpray和大气压化学电离接口非常适合耐受1.2至2毫升/分钟的较高洗脱液流速。这些方法在使用固相或液-液萃取进行净化后应用于生物样品基质。在测定人血浆中的三环胺时，获得了良好的精密度和准确度（分别平均为8.9%和97.7%）。在人尿液中测定苯二氮䓬类药物时，批内和批间平均精密度为9%，平均准确度为95%。检测限在低纳克/毫升范围内。每小时240次进样的一个例子证明了快速LC-MS-MS分析的可行性。
