摘要
目的:建立测定人血浆中替考拉宁浓度的高效液相色谱-紫外检测(HPLC-UV)法,为临床个体化给药提供依据。方法:以哌拉西林钠为内标,将400μL血浆样本采用600μL乙腈沉淀蛋白后,再用二氯甲烷萃取,采用HPLC测定,色谱柱为kromasil柱(150 mm×4.6 mm,5μm),流动相为水(含0.01 mol·L-1磷酸二氢钾,用磷酸调pH至2.84)-乙腈(75∶25,v/v),流速1.0 mL·min^-1,柱温35℃,进样量20μL,检测波长为240 nm。结果:替考拉宁在3.12~100.00μg·mL-1范围内线性关系良好(R2=0.9999),定量下限为3.12μg·mL-1;日内、日间精密度的RSD为0.39%~8.54%,相对偏差为–7.19%~7.00%。血浆样品在经历3次冻融(–20℃到室温)循环、4℃放置6 d和冷冻(–40℃)放置21 d等条件下均稳定,处理后样品在自动进样器中(4℃)放置24 h均稳定(RSD<15%)。测定9例应用替考拉宁患者的血药浓度,仅有2例在有效血药浓度范围。结论:该法操作简便、灵敏、准确,适用于替考拉宁血药浓度的测定。
Objective:To establish a high performance liquid chromatography-ultraviolet(HPLC-UV)method for the determination of teicoplanin in human plasma,and provide evidence for individual therapy.Methods:The internal standard substance was piperacillin sodium.The pretreatment of plasma sample(400μL)included protein precipitation by 600μL acetonitrile and extraction by dichloromethane(CH2Cl2).A kromasil column(150 mm×4.6 mm,5μm)was used.The mobile phase consisted of a mixture of 0.01 mol·L-1 KH2PO4(pH was adjusted to 2.84 with H3PO4)-acetonitrile(75∶25,v/v).The flow rate was 1.0 mL·min^-1.The column temperature was set at 35℃and the sample size was 20μL,the detection wavelength was 240 nm.Results:The concentration of teicoplanin had good linear relation in the range of 3.12-100.00μg·mL-1(R2=0.9999).The low limit of quantitation was 3.12μg·mL-1.RSD of the intra-day and inter-day precision was 0.39%~8.54%.The relative deviation was-7.19%~7.00%.Plasma samples were stable after 3 freeze-thaw cycles(–20℃to room temperature),being laid at 4℃for 6 days and-40℃for 21 days.The pretreated samples were stable in the autosampler(4℃)for 24 h(RSD<15%).Among 9 patients who monitored the concentration of teicoplanin,only 2 of them had the concentration of teicoplanin within the effective range.Conclusion:This method was simple,sensitive and accurate,which was suitable for clinical therapeutic drug monitoring(TDM)of teicoplanin.
作者
王彦改
沈芊
苏甦
王雪梅
姜德春
闫素英
WANG Yan-gai;SHEN Qian;SU Su;WANG Xue-mei;JIANG De-chun;YAN Su-ying(Department of Pharmacy,Xuanwu Hospital,Capital Medical University,Beijing 100053,China)
出处
《中国药物应用与监测》
CAS
2020年第4期226-230,共5页
Chinese Journal of Drug Application and Monitoring
基金
北京市卫生和计划生育委员会老年重大疾病关键技术研究项目(PXM2018_026283_000002)。