Song D, Zhang S, Kohlhof K
Clinical Research Associates, New York, NY 10010, USA.
J Chromatogr B Biomed Appl. 1996 Nov 15;686(2):199-204. doi: 10.1016/s0378-4347(96)00215-0.
A gas chromatographic-negative ion chemical ionization mass spectrometric (GC-NCI-MS) method for the quantitative analysis of clonazepam in human plasma is described. Clonazepam (M(r) = 315) was derivatized by N,O-bis-(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane. A pre-conditioning procedure involving injection of a silyl-8 and ethyl acetate extraction solution from plasma reduces the interaction between clonazepam-TMS and the analytical system. The routine limit of quantification was set to be 0.25 ng/ml with an injection volume of 2 microliters and a sample volume of 1 ml. The signal-to-noise ratio was greater than five. The detection limit for clonazepam can reach 0.1 ng/ml. The isotope clonazepam-d5 was used as the internal standard.
描述了一种用于定量分析人血浆中氯硝西泮的气相色谱 - 负离子化学电离质谱（GC - NCI - MS）方法。氯硝西泮（M(r) = 315）用含1%三甲基氯硅烷的N,O - 双（三甲基硅基）三氟乙酰胺进行衍生化。一种预处理程序，包括从血浆中注入硅烷基 - 8和乙酸乙酯萃取溶液，可减少氯硝西泮 - TMS与分析系统之间的相互作用。常规定量限设定为0.25 ng/ml，进样体积为2微升，样品体积为1毫升。信噪比大于5。氯硝西泮的检测限可达0.1 ng/ml。同位素氯硝西泮 - d5用作内标。
