篇名 | Determination of 5-Fluorouracil in 5-Fluorouracil Injection and Human Serum by HPLC |
---|---|
卷期 | 20:4 |
並列篇名 | 高效液相層析法測定注射液及血清中5-Fluorouracil |
作者 | 祝玲 、 申貴雋 、 丁仕強 、 華欣 |
頁次 | 947-950 |
關鍵字 | high performance liquid chromatography 、 5-FU 、 human serum 、 drug concentration 、 高效液相層析 、 血清 、 濃度 、 MEDLINE 、 Scopus 、 SCIE |
出刊日期 | 201212 |
DOI | 10.6227/jfda.2012200425 |
本研究開發一測定注射液及血清中5-Fluorouracil(5-FU)之高效液
相層析法,層析管柱為Nova-park C18(3.9 × 150 mm, 4.6 μm),移動相為
5 mmol/L磷酸二氫鉀(pH 6.0):甲醇(96:4, v/v),流速為1.0 mL/min,
檢測波長為254 nm,血清經AgNO3(20%)和NaCl(20%)前處理,濃
度範圍0.1-100 μg/mL(R2
= 0.9999)時呈良好線性。 5-FU注射液及血清
中5-FU之最低檢出限量分別為0.10和0.85 μg/mL(S/N = 10),不同濃度的
平均回收率分別為95.79 - 105.1%和90.2 - 108.8%。精密度相對標差RSD為
0.4%,注射液和血清的穩定性和再現性分別小於1.3和2.1%(n = 5)。血清
中之不純物不會產生干擾,以本方法測定5-FU注射液及血清中5-FU具簡
單、快速、敏感且精確等優點。
A high-performance liquid chromatography (HPLC) method was developed for the determination of 5-fluorouracil (5-FU) in 5-FU
injection and human serum. A Nova-park C18 column (3.9 × 150 mm, 4.6 μm) and mobile phase consisting of 5 mmol/L KH2PO4 (pH
6.0) – methanol (96:4, v/v) at a flow rate of 1.0 mL/min were used for separation. The detection wavelength was set at 254 nm. The human
serum was treated with AgNO3
(20%) and NaCl (20%). The method showed a good linear relationship in the range of 0.1 - 100 μg/mL (R2
=
0.9999) with limits of quantification (LOQ) at 0.10 μg/mL and 0.85 μg/mL (S/N = 10) in 5-FU injection and human serum, respectively. The
average recoveries of different concentrations in 5-FU injection and human serum were 95.79 - 105.1% and 90.2 - 108.8%, respectively.
The relative standard deviation (RSD) of precision was 0.4%, and those of stability and repeatability were less than 1.3% and 2.1% (n = 5)
in both samples, respectively. Impurities in the human serum did not interfere with the determination of 5-FU. The method is simple, rapid,
sensitive and can accurately determine 5-FU in 5-FU injection and human serum.