福建农林大学学报(自然科学版)
福建農林大學學報(自然科學版)
복건농림대학학보(자연과학판)
JOURNAL OF FUJIAN AGRICULTURE AND FORESTRY UNIVERSITY(NATURAL SCIENCE EDITION)
2010年
1期
58-62
,共5页
李长流%俞道进%马玉芳%李健%徐敏祥%杨志民%黄一帆
李長流%俞道進%馬玉芳%李健%徐敏祥%楊誌民%黃一帆
리장류%유도진%마옥방%리건%서민상%양지민%황일범
去呋喃甲酰基头孢噻呋%血浆浓度%高效液相色谱法
去呋喃甲酰基頭孢噻呋%血漿濃度%高效液相色譜法
거부남갑선기두포새부%혈장농도%고효액상색보법
desfuroylceftiofur%plasma concentration%HPLC
建立了测定猪血浆中去呋喃甲酰基头孢噻呋(DFC)的高效液相色谱法(HPLC).血浆样品经DTE-磷酸缓冲液提取,过SPE小柱净化浓缩,甲醇洗脱,用XDB-C18色谱柱分离,流动相由乙腈(A)和0.1%三氟乙酸水溶液(B)组成.采用梯度洗脱:0 min为12%A和88%B,15 min为18%A和82%B,18 min为12%A和88%B,平衡至20 min.流速0.8 mL·min~(-1),波长266 nm.以DFC峰面积定量,浓度在0.25-40.0 μg·mL~(-1)时,其峰面积与浓度呈良好的线性关系,r~2=0.9987,平均回收率为82.1%-87.4%,其日内和日间变异系数(RSD)分别为5.04%-8.58%和6.83%-9.34%.该方法适用于血浆中DFC的浓度测定和药代动力学研究.
建立瞭測定豬血漿中去呋喃甲酰基頭孢噻呋(DFC)的高效液相色譜法(HPLC).血漿樣品經DTE-燐痠緩遲液提取,過SPE小柱淨化濃縮,甲醇洗脫,用XDB-C18色譜柱分離,流動相由乙腈(A)和0.1%三氟乙痠水溶液(B)組成.採用梯度洗脫:0 min為12%A和88%B,15 min為18%A和82%B,18 min為12%A和88%B,平衡至20 min.流速0.8 mL·min~(-1),波長266 nm.以DFC峰麵積定量,濃度在0.25-40.0 μg·mL~(-1)時,其峰麵積與濃度呈良好的線性關繫,r~2=0.9987,平均迴收率為82.1%-87.4%,其日內和日間變異繫數(RSD)分彆為5.04%-8.58%和6.83%-9.34%.該方法適用于血漿中DFC的濃度測定和藥代動力學研究.
건립료측정저혈장중거부남갑선기두포새부(DFC)적고효액상색보법(HPLC).혈장양품경DTE-린산완충액제취,과SPE소주정화농축,갑순세탈,용XDB-C18색보주분리,류동상유을정(A)화0.1%삼불을산수용액(B)조성.채용제도세탈:0 min위12%A화88%B,15 min위18%A화82%B,18 min위12%A화88%B,평형지20 min.류속0.8 mL·min~(-1),파장266 nm.이DFC봉면적정량,농도재0.25-40.0 μg·mL~(-1)시,기봉면적여농도정량호적선성관계,r~2=0.9987,평균회수솔위82.1%-87.4%,기일내화일간변이계수(RSD)분별위5.04%-8.58%화6.83%-9.34%.해방법괄용우혈장중DFC적농도측정화약대동역학연구.
High performance liquid chromatography (HPLC) was established to determine desfuroylceftiofur (DFC) in pig plasma. Plasma sample was extracted with dithioerythritol-phosphate buffer, then concentrated and purified by SPE course and eluted with methanol. Chromatographic separation was carried out on a XDB-C18 chromatographic column, the mobile phases consisted of acetonitrile (A) and 0. 1% trifluoroacetic acid solution (B). A gradient elution procedure was performed: 12%A and 88%B at 0 min, 18%A and 82%B at 15 min, 12%A and 88%B at 18 min, then balanced to 20 min. The flow rate was 0. 8 mL·min~(-1), the wave length of DAD detector was 266 nm. The determination was quantitated according to peak area of DFC. The calibration curve was linear in the range of 0. 25-40. 0 μg·mL~(-1) (r~2=0. 9987), and the average recovery was 82. 1%-87. 4%, relative standard deviations (RSD) of inter-day and intra-day were 5. 04%-8. 58% and 6. 83%-9. 34%, respectively. The method could be applied to the concentration determination of DFC in plasma and pharmacokinetics research.