摘要
目的 :建立人血清中盐酸曲马多的高效液相色谱测定法。方法 :采用固相萃取法预处理血清样品 ,分析柱为Symme tryC18柱 (5 μm ,2 5 0mm×4 .6mm) ,流动相为 pH2 .5的 0 .0 2 5mol·L-1磷酸二氢钾缓冲液 乙腈 (82∶18) ,流速为 1.2mL·min-1,荧光检测波长为λex为 2 76nm ,λem为 310nm ,Gain :10 0 ,柱温为 2 5℃。结果 :盐酸曲马多的保留时间为 7.8min左右 ;血药浓度线性范围为 15~ 10 0 0 μg·L-1(r =0 .9999) ,最低检测浓度为 10 μg·L-1(S/N >3) ,萃取回收率在 70 %以上 (n =5 ) ,分析方法回收率在 98%~ 10 1% (n =5 ) ,日内和日间RSD分别为 1.30 %~ 6 .84 %和 1.5 1%~ 3.81% (n =5 )。结论 :本法操作便捷 ,灵敏度和精密度高 ,重现性好 。
OBJECTIVE To establish an HPLC method for determ ination of tramadol hydrochloride in human serum. METHODS Serum samples were pretreated by solid-phase extractio n, then were separated on the Symmetry C 18 column (5 μm,250 mm× 4. 6 mm) at 25℃ with 0.025 mol·L -1 KH 2PO 4 buffer of pH 2.5 - acenitrile(82∶18)as the mobile phase at a flow rate of 1.2 mL·min -1 , and the fluorescence detective wavelength was:λ ex=276 nm and λ em =310 nm, gain was 100.RESULTS Tramadol hydrochloride was eluted at about 7.80 min after injection. Calibration curve of human serum was linear (r= 0.9999 ) in the range of 15~1000 μg·L -1, the detection limit was 10 μg·L -1 (S/N>3),the extraction recovery was more than 70%(n=5), the analyti cal recovery was 98%~101%(n=5), the within-day RSD and between-day RSD were 1.30%~ 6.84% and 1.51%~ 3.81%(n=5)respectively. CONCLUSION The method is simple, sensitive and accurate, and is suitable for the pharmacokinetic study of tramadol hydrochloride.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2004年第6期340-341,共2页
Chinese Journal of Hospital Pharmacy