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目的:建立血浆中 B Z类失能剂的高效液相二极管矩阵检测分析方法,为 B Z类失能剂中毒病人的临床诊断提供分析手段。方法:采用 Sep Pak C18 柱固相提取,乙酸乙酯洗脱, Resolve C18 反相柱分离,0.12% 三氟乙酸( T F A)的 50% 甲醇溶液梯度洗脱,二极管矩阵检测器( D A D) 三波长(220±4)nm ,(254±4)nm ,(300±4)nm 检测。结果:血浆中 H P L C D A D 法检测 4 种失能剂的线性范围为 0.1~1.2 μg,回收率为62.76% ~92.20% ,标准偏差为 3.46% ~11.84% ,最低检出限为 100~400 ng。流动相中 T F A 和甲醇浓度及梯度洗脱是影响分离效果和色谱峰形的主要因素。结论:本文为临床诊断提供简便、快速、灵敏的检测方法,血浆蛋白不干扰测定。4 种失能剂在血浆中采用 H P L C D A D 法同时分离测定目前未见报道。
OBJECTIVE: To establish a HPLC matrix detection and analysis method for plasma BZ-type incapacitating agents, and to provide an analytical method for the clinical diagnosis of BZ-type incapable toxic patients. Methods: The solid phase extraction was performed on a Sep-Pak C18 column, eluted with ethyl acetate, separated on a Resolve C18 reverse phase column and eluted with a gradient of 0.12% trifluoroacetic acid (TFA) in 50% methanol. The diode matrix detector (D A D) three wavelengths (220 ± 4) nm, (254 ± 4) nm, (300 ± 4) nm detection. Results: The linear range of the four kinds of incapacitating agents detected by HPCL-D A D was 0.1-1.2 μg, the recovery was 62.76% -92.20%, and the standard deviation was 3. 46% ~ 11.84%, the lowest detection limit was 100 ~ 400 ng. The mobile phase of T F A and methanol concentration and gradient elution is the main factor affecting the separation and peak shape. Conclusion: This article provides a simple, rapid and sensitive detection method for clinical diagnosis, plasma protein does not interfere with the determination. Four kinds of incapacitating agents in the plasma using H P L C D A D simultaneous determination of the method has not been reported.