Cornpropst J D, Gillespie T A, Shipley L A
Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN 46285, USA.
J Chromatogr B Biomed Appl. 1995 Nov 3;673(1):67-74. doi: 10.1016/0378-4347(95)00238-e.
A method for determining a selective muscarinic agent, LY297802 (compound I), [(3-(3-1-butylthio)-1,2,5-thiadiazol-4-yl)-1-azabicyclo-2.2.2-octa ne], indicated in the treatment of pain, in rat, rabbit, and monkey plasma is described. The analytes, including an internal standard, were extracted from plasma at basic pH with hexane. The organic fraction was evaporated to dryness and the residue reconstituted with mobile phase. The analytes were detected utilizing HPLC in conjunction with electrospray (ES) tandem mass spectrometry (MS-MS). The limit of quantitation was 0.25 ng/ml, and the response was linear to at least 100 ng/ml.
描述了一种在大鼠、兔和猴血浆中测定用于疼痛治疗的选择性毒蕈碱剂LY297802（化合物I），即[(3-(3-丁硫基)-1,2,5-噻二唑-4-基)-1-氮杂双环[2.2.2]辛烷]的方法。包括内标在内的分析物在碱性pH条件下用己烷从血浆中萃取。有机相蒸发至干，残留物用流动相复溶。分析物采用高效液相色谱结合电喷雾（ES）串联质谱（MS-MS）进行检测。定量限为0.25 ng/ml，响应在至少100 ng/ml范围内呈线性。
