吡咯烷二硫代氨基甲酸铵的定性与定量分析  

Study on qualitative identification and quantitative analysis of pyrrolidine dithiocarbamate

作　　者：付恩桃 王秀云[1] 杨鹏[1] 赵鑫[2] 张颖[3] 范国荣[1,2] 

机构地区：[1]福建中医药大学药学院药物制剂教研室,福建福州350108 [2]第二军医大学药学院药物分析学教研室/上海市药物(中药)代谢产物研究重点实验室,上海200433 [3]复旦大学附属华山医院感染科,上海200040

出　　处：《广东药学院学报》2014年第3期327-331,共5页Academic Journal of Guangdong College of Pharmacy

基　　金：国家科技部重大新药创制专项(2011ZX09102-008)

摘　　要：目的建立抗结核病新药吡咯烷二硫代氨基甲酸铵（pyrrolidine dithiocarbamate,PDTC）的定性鉴别与定量分析方法。方法以化学法、紫外光谱（UV）法、红外光谱（IR）法和高效液相色谱（HPLC）法结合对照品进行定性鉴别,采用HPLC法测定PDTC合成产品的质量分数。结果 PDTC水溶液有特征的硫取代显色反应。PDTC 50%（体积分数）甲醇溶液在255、278 nm波长处有最大吸收,在225 nm波长处有最小吸收。PDTC在3 250、2 500 cm-1间出现VSH较强的宽峰,在1 716 cm-1附近为VCS较弱的宽峰。以PDTC对照品为对照,进行PDTC合成产品定量分析,在25.75-206.00μg/mL范围内线性关系良好（r=0.999 8）,低、中、高3个水平的平均加样回收率分别为100.09、100.06%、100.10%,RSD分别为0.59%、1.47%、0.58%（n=3）。结论建立的定性鉴别和定量分析方法准确、可靠、重复性好,可用于PDTC合成产品的质量控制。Objective To establish the method for qualitative identification and quantitative analysis of pyrrolidine dithiocarbamate（PDTC）,a novel anti-tuberculosis agent.Methods PDTC was identified by chemical,ultraviolet（UV） and infrared（IR） spectroscopic methods and high-performance liquid chromatography（HPLC） combined with referrence control.A validated HPLC-UV method was used to determine the content of PDTC synthetic products.Results Chemical tests showed the characteristics of sulfur substituted chromogenic reactions.PDTC in 50% methanol had maximum absorption peaks at 255 nm and 278 nm wavelength.The VSHbroad-peak was strong in the 3 250,2 500 cm-1and the VCc=s Sbroad-peak was weak at 1 716 cm-1.PDTC synthetic product was determined,with the reference substance as control and the linear range of PDTC was 25.75-206.00 μg/mL（r = 0.999 8）.The average recoveries at low, middle and high levels were 100.09%（RSD = 0.59%,n = 3）,100.06%（RSD = 1.47%,n = 3）,100.10%（RSD=0.58%,n= 3）,respectively.Conclution The qualitative and quantitative methods are accurate, reliable and reproducible and could be used for the quality control of PDTC synthetic products.

关 键 词：吡咯烷二硫代氨基甲酸铵 高效液相色谱法 鉴别 含量测定 

分 类 号：R917[医药卫生—药物分析学]