西北药学杂志
西北藥學雜誌
서북약학잡지
2013年
6期
611-613,614
,共4页
钱智磊%周秋云%陆磊%张亮%丁红梓%王洁%林霏申%朱文玉
錢智磊%週鞦雲%陸磊%張亮%丁紅梓%王潔%林霏申%硃文玉
전지뢰%주추운%륙뢰%장량%정홍재%왕길%림비신%주문옥
异烟肼%吡嗪酰胺%利福平%高效液相色谱法
異煙肼%吡嗪酰胺%利福平%高效液相色譜法
이연정%필진선알%리복평%고효액상색보법
isoniazid%rifampicin%pyrazinamide%HPLC
目的:建立快速、灵敏的同时测定人血浆中异烟肼、吡嗪酰胺和利福平的质量浓度的高效液相色谱法。方法血浆样品采用甲醇沉淀蛋白法萃取,采用C18色谱柱(150mm×4.6mm,5.0μm),用甲醇、乙腈、0.05mol·L-1KH2PO3水溶液(三乙胺调pH6.0)进行梯度洗脱,柱温40℃,进样量20μL,采用PDA紫外检测器。结果以峰面积外标法定量,异烟肼在0.20~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9998),吡嗪酰胺在0.20~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9999),利福平胶囊在0.40~25.6μg·mL-1范围内,与峰面积线性关系良好(r=0.9996),回收率为85%~115%,日内、日间精密度RSD均<9.4%(n=5)。结论该方法专属性强、灵敏、准确,适用于同时测定人血浆样品中异烟肼、吡嗪酰胺和利福平的质量浓度。
目的:建立快速、靈敏的同時測定人血漿中異煙肼、吡嗪酰胺和利福平的質量濃度的高效液相色譜法。方法血漿樣品採用甲醇沉澱蛋白法萃取,採用C18色譜柱(150mm×4.6mm,5.0μm),用甲醇、乙腈、0.05mol·L-1KH2PO3水溶液(三乙胺調pH6.0)進行梯度洗脫,柱溫40℃,進樣量20μL,採用PDA紫外檢測器。結果以峰麵積外標法定量,異煙肼在0.20~25.6μg·mL-1範圍內,與峰麵積線性關繫良好(r=0.9998),吡嗪酰胺在0.20~25.6μg·mL-1範圍內,與峰麵積線性關繫良好(r=0.9999),利福平膠囊在0.40~25.6μg·mL-1範圍內,與峰麵積線性關繫良好(r=0.9996),迴收率為85%~115%,日內、日間精密度RSD均<9.4%(n=5)。結論該方法專屬性彊、靈敏、準確,適用于同時測定人血漿樣品中異煙肼、吡嗪酰胺和利福平的質量濃度。
목적:건립쾌속、령민적동시측정인혈장중이연정、필진선알화리복평적질량농도적고효액상색보법。방법혈장양품채용갑순침정단백법췌취,채용C18색보주(150mm×4.6mm,5.0μm),용갑순、을정、0.05mol·L-1KH2PO3수용액(삼을알조pH6.0)진행제도세탈,주온40℃,진양량20μL,채용PDA자외검측기。결과이봉면적외표법정량,이연정재0.20~25.6μg·mL-1범위내,여봉면적선성관계량호(r=0.9998),필진선알재0.20~25.6μg·mL-1범위내,여봉면적선성관계량호(r=0.9999),리복평효낭재0.40~25.6μg·mL-1범위내,여봉면적선성관계량호(r=0.9996),회수솔위85%~115%,일내、일간정밀도RSD균<9.4%(n=5)。결론해방법전속성강、령민、준학,괄용우동시측정인혈장양품중이연정、필진선알화리복평적질량농도。
Objective To develop an HPLC method for the simultaneous determination of isoniazid ,rifampicin and pyrazinamide in human plasma .Methods The compounds and internal standard were extracted from the plasma by a protein precipitation procedure with methanol .The separation of the analytes was performed on a C18 column (150 mm × 4 .6 mm ,5 .0μm) at 40 ℃ ,using a gra-dient elution program with solvents consisting of methanol ,acetonitrile and 0.05 mol · L -1 KH2 PO3-H2O .The injection volume was 20 μL .The compounds were detected by PDA .Results Calibration curves in spiked plasma were linear at 0 .20-25 .6 ,0.20-25 .6 and 0 .40-25 .6 μg · mL - 1 for isoniazid ,rifampicin and pyrazinamide ,respectively .The recoveries were 85% ~115% ,and the intra-day and inter-day RSDs were <9 .4% .Conclusion The method is specific ,sensitive and accurate ,and it can be used for the simultaneous determination of isoniazid ,rifampicin and pyrazinamide in human plasma .