安徽医药
安徽醫藥
안휘의약
ANHUI MEDICAL AND PHARMACEUTICAL JOURNAL
2014年
8期
1433-1436
,共4页
俞敏%王世亮%王小董%陈蒙蒙
俞敏%王世亮%王小董%陳矇矇
유민%왕세량%왕소동%진몽몽
氟尿嘧啶植入剂%血药浓度%高效液相色谱法
氟尿嘧啶植入劑%血藥濃度%高效液相色譜法
불뇨밀정식입제%혈약농도%고효액상색보법
fluorouracil implants%plasma concentration%HPLC
目的:建立测定人血浆中5-氟尿嘧啶(5-Fu)浓度的方法。方法以5-溴尿嘧啶(5-Bru)为内标,硫酸铵为蛋白沉淀剂,血浆采用乙酸乙酯提取处理后以高效液相色谱法进样测定,其中,色谱柱为Hypersil ODS2(5μm,4.6 mm ×250 mm),流动相为甲醇∶水(5∶95,V/V)溶液,流速0.8 mL·min-1,检测波长为266 nm,柱温为25℃。结果在0.020~0.250 mg·L-1浓度范围内药物浓度与响应值之间线性关系良(r=0.9996),最低定量限浓度为0.020 mg·L-1,日内和日间RSD分别为2.97%~11.17%、1.67%~5.47%;高、中、低浓度的方法回收率均高于96%,高、中、低浓度的提取回收率均高于70%。血浆样品在室温24 h内及冷冻条件下20 d内稳定性良好。结论该方法具有操作简便可靠、准确、稳定性高等特点,适用于氟尿嘧啶植入剂人血浆中5-Fu浓度的测定。
目的:建立測定人血漿中5-氟尿嘧啶(5-Fu)濃度的方法。方法以5-溴尿嘧啶(5-Bru)為內標,硫痠銨為蛋白沉澱劑,血漿採用乙痠乙酯提取處理後以高效液相色譜法進樣測定,其中,色譜柱為Hypersil ODS2(5μm,4.6 mm ×250 mm),流動相為甲醇∶水(5∶95,V/V)溶液,流速0.8 mL·min-1,檢測波長為266 nm,柱溫為25℃。結果在0.020~0.250 mg·L-1濃度範圍內藥物濃度與響應值之間線性關繫良(r=0.9996),最低定量限濃度為0.020 mg·L-1,日內和日間RSD分彆為2.97%~11.17%、1.67%~5.47%;高、中、低濃度的方法迴收率均高于96%,高、中、低濃度的提取迴收率均高于70%。血漿樣品在室溫24 h內及冷凍條件下20 d內穩定性良好。結論該方法具有操作簡便可靠、準確、穩定性高等特點,適用于氟尿嘧啶植入劑人血漿中5-Fu濃度的測定。
목적:건립측정인혈장중5-불뇨밀정(5-Fu)농도적방법。방법이5-추뇨밀정(5-Bru)위내표,류산안위단백침정제,혈장채용을산을지제취처리후이고효액상색보법진양측정,기중,색보주위Hypersil ODS2(5μm,4.6 mm ×250 mm),류동상위갑순∶수(5∶95,V/V)용액,류속0.8 mL·min-1,검측파장위266 nm,주온위25℃。결과재0.020~0.250 mg·L-1농도범위내약물농도여향응치지간선성관계량(r=0.9996),최저정량한농도위0.020 mg·L-1,일내화일간RSD분별위2.97%~11.17%、1.67%~5.47%;고、중、저농도적방법회수솔균고우96%,고、중、저농도적제취회수솔균고우70%。혈장양품재실온24 h내급냉동조건하20 d내은정성량호。결론해방법구유조작간편가고、준학、은정성고등특점,괄용우불뇨밀정식입제인혈장중5-Fu농도적측정。
Objective To develop a method for the determination of 5-fluorouracil concentration in human plasma.Methods 5-Bro-mouracil was used as the internal standard,ammonium sulfate was added to precipitate protein,plasma sample was treated with extrac-tion of ethyl acetate,and then HPLC method was adopted for concentration determination.The determination was performed on Hypersil ODS2 (5 μm,4.6 mm ×250 mm)column with mobile phase consisting of methyl alcohol-water (5∶95,v/v)at the flow rate of 0.8 mL ·min-1 .The detection wavelength was set at 266 nm and column temperature was 25℃.Results The linear range of 5-fluorouracil was 0.020~0.250 mg·L-1 (r=0.999 6).The lowest limit of quantification was 0.020 mg·L-1 .The RSD of intra-day and inter-day were 2.97%~11.17% and 1.67%~5.47%respectively.The recovery rates were all higher than 96%at high,medium and low con-centrations.The extraction rates were all higher than 70% at high,medium and low concentrations.The plasma samples were stable within 24 hours at room temperature and within 20 days in frozen condition.Conclusions This method is simple,precise and stable, which is suitable for the determination of 5-fluorouracil concentration in human plasma.