摘要
目的:建立同时快速测定血浆中更昔洛韦、阿昔洛韦、喷昔洛韦浓度的方法。方法:血浆经AccuBOND ODS-C_(18)固相萃取小柱净化富积后,采用HPLC法进行测定。色谱柱:Sinochrom ODS-BP(250mm×4.6mm,5μm),柱温:40℃,流动相:0.015mol·L^(-1)磷酸二氢钠(稀磷酸调pH 3.14)-甲醇(90:10),流速:1.0mL·min^(-1),荧光检测波长:λ_(ex)=270nm,λ_(em)= 373nm,内标物:鸟嘌呤。结果:血浆内源性杂质对样品测定无干扰,3组分在10min以内全部洗脱完毕并能完全分离。更昔洛韦、阿昔洛韦、喷昔洛韦的线性方程测定分别为:Y=0.024947+0.084400C(r=0.9992),Y=0.016342+0.078968C(r= 0.9999),Y=0.038859+0.44034C(r=0.9998);线性范围分别为0.10～50.0,0.10～50.0,0.04～20.0μg·mL^(-1);检测限(S/ N=3)分别为0.05,0.05,0.01μg·mL^(-1);各组分提取回收率均大于70%,方法回收率在90%～110%之间,日内和日间精密度的RSD均小于6%。结论:本法简便、快速、灵敏、准确,可用于核苷类抗病毒药的体内分析及临床药学研究。
Objective ：To develop a rapid and simple HPLC method for the simultaneous determination of aciclovir, ganciclovir and penciclovir in plasma. Methods：After being purified by solid phase extraction cartridges, samples were achieved and separated by a C18 column with a mobile phase of 0. 015 mol· L^-1 phosphate buffer（ adjusted to pH 3. 14 with dilute phosphoric acid） -CH3OH（90： 10）at a flow- rate of 1.0 mL·min^-1, temperature set at 40 ℃, and measured by fluorescence detection using an excitation wavelength of 270 nm and an emission wavelength of 373 nm. Guanine was chosen as the internal standard. Results：The drug-free plasma did not interfere with the drugs and internal standard, all components were eluted in 10 minutes and separated each other. The linear equations were Y = 0. 024947 ＋ 0. 084400C （ r = 0. 9992 ） for ganciclovir, Y = 0. 016342 ＋ 0. 078968 C （ r = 0. 9999 ） for aciclovir and Y = 0. 038859 ＋ 0. 44034C （ r = 0. 9998 ） for penciclovir, respectively. The linearity ranged from 0. 1 to 50. 0 μg · mL^-1 for both ganciclovir and aciciovir and from 0. 04 to 20. 0 μg· mL^-1 for penciclovir, respectively. At a signal - to - noise ratio of 3 ： 1, the detection limit was 0. 05 μg ·mL^-1 for both ganciclovir and aciclovir and 0.01 μg·mL^-1 for penciclovir, respectively. The extraction recoveries of these drugs were all higher than 70% and method recoveries varied from 90% to 110 %. The precisions （RSD）of within - day and between - day were all less than 6%. Conclution： This methond is simple, rapid, accurate and sensitive. It can be used to determine the concentrations of ganciclovir, aciclovir and penciclovir in plasma simultaneously and rapidly, and can be applied to the clinical pharmaceutical research in vivo.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第9期1199-1203,共5页
Chinese Journal of Pharmaceutical Analysis
基金
山西省自然科学基金资助(No.20031104)
