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1,4-苯二氮(艹卓)化合物(BDZs)二氮(艹卓)环上1,2,3位的结构差异可显著影响300~500nm 的光谱带。采用一阶和二阶导数紫外光潜(△_1和△_2)法可在合适 pH 条件下对BDZs(Ⅲ:利眠宁,Ⅳ:去甲羟安定,Ⅴ:安定,Ⅵ:去甲安定)及相关二苯酮(Ⅰ:2-氨基5-氯-二苯酮,Ⅱ:2-甲氨基-5-氯-二苯酮)混合物中的单一化合物进行选择性测定。尿液的提取取适量Ⅰ~Ⅵ的甲醇溶液与15g NaCl 加入60ml 尿液中,涡流振荡,氯仿提取(20ml×3),总有机相以 Na_2SO_4脱水、干燥,残渣加1.5ml 甲醇溶解,取甲醇液250μl 稀释至750μl,按下述方法对各化合物作定量测定。总混合物测定基于△_2,在中性甲醇中于450nm 对Ⅰ、Ⅱ定量、定性分析,BDZs不干扰;在中性溶液中于380.5nm 处测定Ⅲ,其它化合物在此波长处无明显吸收;中性和酸性(0.01mol/L HCl)甲醇溶液中Ⅳ,Ⅴ及Ⅵ有相似的定性(峰位置)及定量(摩尔
The structural differences at 1, 2 and 3 positions of 1,4-benzodiazepine (BDZs) diazepam ring can significantly affect the spectral band of 300-500 nm. BDZs (Ⅲ: Chlordiazepoxide, Ⅳ: norcoxetine, Ⅴ: diazepam, Ⅵ: norfluazolam) were prepared using the first and second derivative ultraviolet light latent (△ _1 and △ _2) And related benzophenone (Ⅰ: 2-amino 5-chloro-benzophenone, Ⅱ: 2-methylamino-5-chloro-benzophenone) mixture of compounds for selective determination. Extraction of urine The appropriate amount of methanol solution Ⅰ ~ Ⅵ and 15g NaCl was added to 60ml of urine, vortexed, extracted with chloroform (20ml × 3), the total organic phase was dried over Na_2SO_4, dried, the residue was dissolved in methanol 1.5ml, methanol 250 μl of the solution was diluted to 750 μl, and the compounds were quantitatively determined as follows. The total mixture was determined based on △ _2, qualitative and quantitative analysis of Ⅰ, Ⅱ at 450 nm in neutral methanol, without interference of BDZs; Ⅲ at 380.5 nm in neutral solution; no significant absorption of other compounds at this wavelength; Similar qualitative (peak position) and quantification (molar) concentrations of IV, V and VI in both acidic and acidic (0.01 mol / L HCl)