高效液相色谱法测定人血清中5-氟尿嘧啶的浓度

目的：测定 ５－氟尿嘧啶在人血清中的浓度。方法：三氯乙酸沉淀血清中蛋白质，高效液相色谱法测定含量。色谱柱为 ＳｈｉｍｐａｃｋＣＬＣ Ｃ１８柱，加 ＹＷＧ预柱；流动相为 ０．２５％磷酸二氢钾－乙腈（９８：２），ｐＨ７．０；流速为 １ｍｌ／ｍｉｎ；紫外检测波长 ２６５ｎｍ。分别在低浓度范围（０．１９５～６．２５０μｇ／ｍｌ）和高浓度范围（６．２５０～２００．００μｇ／ｍｌ）制作标准曲线以用于定量。结果：５－氟尿嘧啶在 ０．１９５～２００μｇ／ｍｌ浓度范围呈良好的线性关系，０．８、４、２０和１００μｇ／ｍｌ４个浓度点的日内平均回收率和ＲＳＤ分别为１０４．８８％、１．９５％，１０４．５８％、１．３８％，１０１．４０％、０．３９％，９９．１４％、０．３７％；日间平均回收率和ＲＳＤ分别为１０５．１２％、２．０２％，１０６．３０％、０．７８％，１００．６０％、０．６５％，９９．３８％、０ ９２％。结论：本文建立的方法快速、准确，适合于５－氟尿嘧啶的药代动力学研究和常规血药浓度监测。

Determination of Fluorouracil in Human Serum With HPLC

OBJECTIVE: To determine the content of 5-Fu in human serum.METHODS: Serum protein was precipitated with trichloroacetic acid .HPLC was used for determination of 5-Fu .The column was Shimpack CLC C18(150 × 6mm, 5μm)with YWG for protection.The mobile phase was 0.25% KH2PO4-acetonitrile(98: 2, pH7.0) .The flow rate was 1ml/min.The detection wavelength was 265nm.Two standard curves were made in the concentrations of 0.195～6.250μg/ ml and 6.25～200.00μg/ml, respectively.RESULTS: The calibration curves revealed linearity in the range of 0.195～200μg/ml.The with-in-day recoveries and RSDs of 5-Fu at 0.8, 4, 20 and 100μg/ ml concentration points were 104. 88%, 1.95%; 104.58%,1.38%; 101.40%, 0.39%and 99.14%, 0.37%, and the between-day recoveries and RSDs of 5-Fu were 105.12%, 2.02%;106.30 %, 0.78 %; 100.60 %, 0.65 % and 99.38 %, 0.92 % respectively. CONCLUSION: This method is rapid, accurate and suitable for pharmacokinetical study and conventional monitoring of 5-Fu.