高效液相層析法測定注射液及血清中 5-Fluorouracil   全文下載

Determination of 5-Fluorouracil in 5-Fluorouracil Injection and Human Serum by HPLC

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.