Macfarlane R G, Midgley J M, Watson D G, Evans P D
Department of Pharmacy, University of Strathclyde, Glasgow, Scotland, U.K.
J Chromatogr. 1990 Oct 26;532(1):13-25. doi: 10.1016/s0378-4347(00)83747-0.
The N-acetylated metabolites of p-tyramine, p-octopamine and dopamine were identified unambiguously and quantitatively determined in a single ventral thoracic nerve cord of the locust, Schistocerca gregaria, by gas chromatography-negative-ion chemical ionisation mass spectrometry (GC-NICIMS). Deuterium-labelled analogues of each compound were added to a single ventral thoracic nerve cord in acetonitrile: the tissue was homogenised and the suspension centrifuged. The solvent was removed from the supernatant and the resultant residue was derivatised with trifluoroacetic anhydride. Under negative-ion chemical ionisation conditions, the trifluoroacetyl derivatives produced ions which were sufficiently abundant to be suitable for selected-ion monitoring. This method is highly specific and gave a limit of detection below the picogram levels. N-Acetyl-5-hydroxytryptamine was determined using a previously published GC-NICIMS technique [S.P. Markey, R.W. Colburn and J.N. Johannessen, Biomed. Mass Spectrom., 7 (1981) 301]. The concentrations of N-acetyltyramine, N-acetyloctopamine, N-acetyldopamine and N-acetyl-5-hydroxytryptamine in locust thoracic nerve cords were, respectively, 1.86 +/- 0.71, 1.13 +/- 0.34, 6.77 +/- 8.48 and 0.07 +/- 0.02 ng per tissue.
通过气相色谱 - 负离子化学电离质谱法(GC - NICIMS),在沙漠蝗(Schistocerca gregaria)的单条腹侧胸神经索中明确鉴定并定量测定了对酪胺、对章鱼胺和多巴胺的N - 乙酰化代谢产物。将每种化合物的氘标记类似物加入到乙腈中的单条腹侧胸神经索中:将组织匀浆并将悬浮液离心。从上清液中除去溶剂,所得残渣用三氟乙酸酐衍生化。在负离子化学电离条件下,三氟乙酰衍生物产生的离子丰度足以适用于选择离子监测。该方法具有高度特异性,检测限低于皮克水平。使用先前发表的GC - NICIMS技术[S.P. Markey,R.W. Colburn和J.N. Johannessen,Biomed. Mass Spectrom.,7(1981)301]测定N - 乙酰 - 5 - 羟色胺。蝗虫胸神经索中N - 乙酰酪胺、N - 乙酰章鱼胺、N - 乙酰多巴胺和N - 乙酰 - 5 - 羟色胺的浓度分别为每组织1.86±0.71、1.13±0.34、6.77±8.48和0.07±0.02纳克。