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高效液相色谱法测定人乳汁中枸橼酸芬太尼浓度
Determination of Fentanyl in the Breast Latex of Caesarean Women After Patient-Control Analgesia by HPLC
【摘要】 目的建立剖宫产产妇乳汁中枸橼酸芬太尼浓度测定的HPLC方法,并考察剖宫产产妇应用枸橼酸芬太尼镇痛泵镇痛后,芬太尼在乳汁中的分布情况,探讨剖宫产术后新生儿的合理哺乳时间。方法1mL乳汁中加入0.5mol·L-1NaOH200μL碱化,涡旋30s,再加入环己烷5mL,涡旋2min,于2000r·min-1离心20min,静置10min,取上述有机相4mL于另一干净试管中,在N2流下吹干,残渣用流动相350μL溶解,进样量100μL。采用AgillentZorbaxSB-C18柱(4.6mm×250mm,5μm),以0.015mol·L-1磷酸二氢钠-乙腈(60∶40)为流动相,流速为0.7mL·min-1,于200nm波长下检测。结果枸橼酸芬太尼在40~2000μg·L-1内线性关系良好(r=0.9997),方法回收率为85.3%~101.6%,乳汁低、中、高3种浓度的萃取回收率(n=5)分别为62.7%,66.3%,65.6%;RSD(n=5)分别为8.11%,6.72%,4.83%;方法回收率(n=5)分别为86.1%,96.4%,103.7%,日内和日间精密度RSD小于12%。结论本法操作简单,灵敏,准确,重现性好,能满足临床对芬太尼乳药浓度的测定,可用于芬太尼在乳汁中的浓度分布研究。
【Abstract】 OBJECTIVE To develop a simple HPLC method for the determination of fentanyl in the breast milk of caesarean women after patient-control analgesia.METHODS 200 μL of NaOH(0.5 mol·L-1 ) was added into 1 mL human milk.After the sample was extracted by 5 mL of cyclohexane,4 mL organic layer was transferred to a clean tube and evaporated to dryness under a continues nitrogen stream in a waterbath at 40 ℃.The residuel was reconstituted in 350μL of mobile phase and 100μL was injected into an Agillent SB-C18 HPLC column(4.6 mm × 250 mm , 5 μm).The mobile phase consisted of 0.015 mol·L-1NaH2PO4-acetonitrile(60∶40)at a flow rate of 0.7 mL·min-1 .The detection wavelength was 200 nm.RESULTS The linear range was 40-2 000 μg·L-1(r=0.999 7), and the limit of determination was 125 μg·L-1.extraction recoveries of low, medium and high concentration were 62.7%,66.3% and 65.6%.The method recoveries were 86.1%,96.4% and 103.7%,and the RSDs of within-day and between-day were below 12%.CONCLUSION This method is simple, sensitive for the determination of fentanyl in the milk of cesarean women after patient-control analgesia, it is applicable for the pharmacokinetic study of fentanyl.
- 【文献出处】 中国药学杂志 ,Chinese Pharmaceutical Journal , 编辑部邮箱 ,2009年13期
- 【分类号】R96
- 【被引频次】6
- 【下载频次】149