摘要
目的 建立使用离子对反相高效液相色谱测定吉西他滨血药浓度的方法。方法 血浆用三氯乙酸沉淀后取上清液直接进样。色谱柱为SymmetryC18(4 6mm× 2 5 0mm ,5 μm) ,流动相为 0 5 2 %的磷酸二氢钠溶液 (pH 2 6 6 ) 乙腈 (85 :15 ,含 0 2 0 2 %庚烷磺酸钠 )。柱温 2 5℃ ,流速 1 0mL·min-1,检测波长 2 73nm。结果 吉西他滨血药浓度在 0 1～ 10 0 μg·mL-1内的线性关系良好 (r =0 9999) ,血浆中低、中、高 3种浓度的方法回收率在 97 39%～ 10 3 11%之间 ,日内RSD≤ 1 94 % ,日间RSD≤ 7 34%。结论 本法快速、灵敏、高效 。
OBJECTIVE: To establish a ion-pair RP-HPLC method for the determination of gemcitabine in human plasma. METHODS: Samples were prepared by protein precipitation. The column was Waters Symmetry C18(4.6 mm × 250 mm, 5 μm) and the temperature was set at 25°C . The mobile phase was 0.52% phosphate buffer (pH 2.66)-acetonitrile (85:15) containing 0.202% sodium 1-heptanesulfonate and the flow rate was 1.0 mL·min-1. The detection wavelength was at 273 nm. RESULTS: The range of calibration curve was 0.1 ∼ 100 μg· mL-1 (r = 0.999 9). The recovery of low, medium and high concentration were within 97.39% ∼ 103.11%. The RSD of intra-run and inter-run did not exceed 1.94% and 7.34% respectively. CONCLUSION: The method is rapid, sensitive and efficient.
出处
《中国药学杂志》
EI
CAS
CSCD
北大核心
2005年第4期295-296,307,共3页
Chinese Pharmaceutical Journal
基金
浙江省医药卫生科学研究基金资助 (2 0 0 4A0 2 8)
关键词
吉西他滨
反相高效液相色谱法
离子对
血浆
Acetonitrile
High performance liquid chromatography
Ions
Precipitation (chemical)
Proteins
Thermal effects
Water
