摘要
目的采用HPLC法测定癌症患者盐酸二甲双胍的血药浓度。方法采用乙腈沉淀蛋白,制备样品,内标为阿替洛尔,采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-10 mmol·L^-1磷酸二氢钾水溶液(31∶69,内含6 mmol·L^-1十二烷基磺酸钠、0.5%三乙胺,用磷酸调pH3.5),流速1.0 mL·min^-1,波长236 nm,柱温40℃。结果0.625~20μg·mL^-1盐酸二甲双胍的线性关系良好,标准曲线方程为:Y=0.9349X-0.1386(r^2=0.9994),最低检测限为0.325μg·mL^-1,方法回收率为94.13%~105.13%,RSD≤6.2%;提取回收率为76.33%~81.81%,RSD≤7.7%。日内、日间RSD≤6.2%,室温(25℃)放置8 h、反复冻融3次、冷冻7 d稳定性的RSD≤8.9%。结论所用方法运行时间短、消耗溶剂少、分离度好、灵敏度高,适用于癌症患者盐酸二甲双胍血药浓度的测定。
OBJECTIVE To establish an HPLC method for the determination of metformin hydrochloride in blood from cancer patients.METHODS Samples were prepared by precipitation of protein with acetonitrile.Atenolol was chosen as internal standard.Diamonsil C18(250 mm×4.6 mm,5μm)column was adopted,and the mobile phase was acetonitrile-10 mmol·L^-1 potassium dihydrogen phosphate solution(31∶69,containing 6 mmol·L^-1 Sodium dodecyl sulfonate),0.5%triethylamine,pH adjusted to 3.5 with phosphoric acid.Flow rate was 1.0 mL·min^-1 with detection wavelength of 236 nm and the column temperature of 40℃.RESULTS Quantitative linearity of metformin hydrochloride was good in the range of 0.625-20μg·mL^-1.The standard curve equation was Y=0.9349X-0.1386(r^2=0.9994).The minimum detection limit was 0.325μg·mL^-1,and the recovery of the method was 94.13%-105.13% with RSD≤6.2%.The extraction recovery of metformin hydrochloride was 76.33%-81.81% with RSD≤7.7%.Intraday and daytime were good with RSD≤6.2%.Samples were placed at the room temperature(25℃)for 8 hours,resulting in RSD≤6.2% for intraday and daytime.The freeze-thaw cycles were repeated three times,and the RSD of the 7-day stability was≤8.9%.CONCLUSION This method has short running time,less solvent consumption,good resolution and high sensitivity.It is suitable for the determination of metformin hydrochloride in cancer patient blood.
作者
任赛赛
李德强
袁叶
贡莹
刘剑
杨爽爽
张志清
REN Saisai;LI Deqiang;YUAN Ye;GONG Ying;LIU Jian;YANG Shuangshuang;ZHANG Zhiqing(Department of Pharmacy,Second Hospital of Hebei Medical University,Shijiazhuang,Hebei,050000 P.R.China;School of Pharmacy,Hebei Medical University,Shijiazhuang,Hebei,050017 P.R.China)
出处
《华西药学杂志》
CAS
CSCD
2020年第1期54-58,共5页
West China Journal of Pharmaceutical Sciences
关键词
盐酸二甲双胍
高效液相色谱法
血药浓度
阿替洛尔
癌症患者
浓度监测
特殊人群
预防癌症
Metformin hydrochloride
HPLC
Plasma concentration
Atenolol
Cancer patient
Concentration monitoring
Special population
Prevention of cancer
