摘要
采用液相色谱-质谱法测定指纹汗液中咖啡因及其代谢物副黄嘌呤的含量。指纹汗液用润湿的滤纸提取后，加入甲醇，在35℃下超声3min。用Thermo Gold ODSC18色谱柱分离，用甲醇与冰乙酸（0．2＋99．8）溶液以体积比65比35组成的混合液洗脱，采用正离子模式监测。咖啡因及副黄嘌呤在一定的浓度范围内与其峰面积呈线性关系，方法的检出限（3S／N）分别为0．3，1．7ng·片-1。加标回收率在65．5％～71．3％之间，测定值的相对标准偏差在3．3％～14％之间。指纹汗液中咖啡因的检出时间从服用咖啡因后1h开始，一直持续到14h，副黄嘌呤检出时间从服用3h后持续到14h。
LC-MS was applied to the determination of caffeine and its major metabolite paraxanthine in fingerprint sweat. Fingerprint sweat was extracted ultrasonically with methanol from wet filter paper for 3 min at3 5 ℃. Thermo Gold ODS C18 column was used as stationary phase,and a mixture of methanol and acetic acid（ 0. 2 ＋ 99. 8） solution（ 65 ＋ 35） was used as mobile phase. Positive electrospray ionization was used in the detection. Linear relationships between values of peak area and concentration of caffeine and paraxanthine were kept in definite ranges,with detection limits（ 3 S / N） of 0. 3,1. 7 ng · 片- 1,respectively. Values of recovery found by standard addition method were in the range of 6 5. 5 %- 7 1. 3 %,and values of RSD＇ s in the range of 3.3 %- 1 4 %. Caffeine in fingerprint sweat could be detected from 1 h to 1 4 h after taking caffeine, and paraxanthine could be detected from 3 h to 1 4 h.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2015年第6期795-799,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
