摘要
联用选择性耗尽进样和胶束扫集两种在线富集技术,建立了尿样中麻黄碱和可待因含量测定的灵敏方法,并通过日内、日间、柱间实验考察了方法的稳定性。胶束扫集电动色谱缓冲体系为80mmol/L十二烷基磺酸钠(SDS)-20mmol/LNaH2PO4(pH2.20)-18%乙腈(V/V),分离电压-20kV,进样电压10kV,进样时间150s,测量波长200nm。同时讨论了pH值、SDS浓度、选择性耗尽进样萃取液电导、进样电压、进样时间和进水长度等对分离效果的影响。结果显示,方法富集功能很强,对麻黄碱和可待因含的富集倍数分别达5800和2490以上。在优化条件下,方法线性关系良好(r=0.9999),麻黄碱和可待因的线性范围分别为0.500～16.0μg/L和2.00～48.0μg/L,检出限分别为0.10和0.80μg/L。方法稳定性良好,日内、日间和柱间的RSD分别为2.6%,5.9%和6.6%。应用于实际尿样分析,回收率在96.8%～106%之间,RSD≤4.7%,结果比较满意。
Two online preconcentration techniques including cation-selective exhaustive injection（CSEI）, and sweeping mieellar electrokinetie chromatography （sweep-MEKC） were used in determination of Ephedrine （Ep） and Codeine （Code） in human urine. Stability was also evaluated by intra-day, inter-day and intercolumn experiment. The separation buffer contained 80 mmol/L SDS, 20mmol/L NaH2PO4 （pH = 2.20） , and 18% ACN（V/V）. The sample was injected at 10 kV for 150 s, separated at -20 kV, and detected at 200 nm. Effects of pH, SDS concentration, and condeuctivity of extraction buffer, injection voltage, injection time, water zone length on the separation were discussed. The result showed that, sensitivity enhancement of Ep and Code were above 5800 and 2490 times by CSEI-sweeping. During method validation, calibration plots were linear（r =0.9999） over a range of 0.5 -48 μg/L, and the LODs were 0.10μg/L for Ep and 0. 80 μg/L for Co. Under the optimum conditions, good stability was obtained with, RSD ≤2. 6% for intraday（ n = 5）, RSD ≤5.9% for inter-day（ n = 7 ）, and RSD ≤ 6.6% for inter-column （ n = 3 ）. Furthermore, this method was successfully applied for the dectection of Ep and Code in human urine with the recoverities of 96. 8% -106%, and RSDs ≤4. 7%.
出处
《分析化学》
SCIE
CAS
CSCD
北大核心
2009年第8期1137-1141,共5页
Chinese Journal of Analytical Chemistry
基金
广西自然科学基金(No.0481019)
'5广东科贸学院院级课题(No.GDKM2009-25)资助
关键词
选择性耗尽进样
胶束扫集电动色谱
麻黄碱
可待因
人尿
Cation-selective exhaustive injection, sweeping micellar electrokinetie chromatography, ephedrine, codeine, urine
