摘要
目的建立测定人血浆中拉莫三嗪药物浓度的中心切割二维液相色谱法。方法采用外标法定量,第一维色谱柱:SNCB(T)-1A(硅胶,4.6 mm×50 mm,5µm),流动相A:VCV-1D移动相,流速:0.4 ml/min;流动相B:水,流速:1.0ml/min;第二维色谱柱:Symmetry C_(18)(4.6 mm×250 mm,5µm),流动相:乙腈-10 mmol/L乙酸铵溶液(V/V=25∶75),流速:1.0ml/min;中间色谱柱:SBX4-MA(树脂,3.0 mm×10 mm,5µm);紫外检测波长306 nm,柱温:45℃,进样量:200µl。结果拉莫三嗪在1.24~39.50µg/ml血药浓度范围内线性关系良好(r=0.9999),定量下限为1.24µg/ml,检测限为0.02µg/ml;日内精密度RSD均小于5%,日间精密度RSD均小于10%;日内准确度范围为102.17%~111.17%,日间准确度范围为99.80%~107.31%;回收率RSD均小于5%,其变化范围在89.95%~96.16%;经室温保存24 h、反复冻融3次和-40℃保存2周等稳定性考察,其测定值/标示值比值范围在87.01%~115.88%。结论本研究建立的方法操作简单、稳定性好、灵敏度高、重现性好,适用于临床开展拉莫三嗪血药浓度监测工作,为临床个体化用药指导提供可靠的监测数据支持。
Objective To establish a central cutting two-dimensional liquid chromatography for the determination of lamotrigine in human plasma.Methods External standard method was used.The first dimensional chromatographic column:SNCB(T)-1A(silica gel,4.6 mm×50 mm,5μm),mobile phase A:VCV-1D mobile phase,flow rate:0.4 ml/min;mobile phase B:water,flow rate:1.0 ml/min;second dimensional chromatographic column:Symmetry C_(18)(4.6 mm×250 mm,5μm),mobile phase:acetonitrile-10 mmol/L ammonium acetate solution(V/V=25∶75),flow rate:1.0 ml/min;Intermediate column:SBX 4-MA(resin,3.0 mm×10 mm,5μm).The UV detection wavelength:306 nm,the column temperature:45℃,and the injection volume:200μl.Results The linear range of lamotrigine was 1.24-39.50μg/ml,the lower limit of quantification was 1.24μg/ml,the detection limit was 0.02μg/ml,the intra-day precision RSD was less than 5%,the day-to-day precision RSD was less than 10%,the variation of intra-day accuracy ranged from 102.17%to 111.17%,and the daytime accuracy variation ranged from 99.80%to 107.31%the recovery RSD was less than 5%,and the variation range was 89.95%-96.16%.After 24 hours storage at room temperature,repeated freezing and thawing for 3 times and storage at−40℃for 2 weeks,the ratio of the measured value/labeled value ranged from 87.01%to 115.88%.Conclusion In this study,a method with simple operation,good stability,high sensitivity and good reproducibility was established,which could be suitable for clinical monitoring of blood concentration of lamotrigine and provide reliable monitoring data support for clinical individualized medication guidance.
作者
林君容
张敏新
赵雪梅
黄爱文
LIN Junrong;ZHANG Minxin;ZHAO Xuemei;HUANG Aiwen(Department of Clinical Pharmacy,No.900 Hospital of Joint Logistic Support Force,Fuzhou 350025,China)
出处
《药学实践与服务》
2026年第1期53-58,共6页
Journal of Pharmaceutical Practice and Service
关键词
拉莫三嗪
血药浓度
二维液相色谱
中心切割
lamotrigine
plasma concentration
two-dimensional liquid chromatography
central cutting
