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作 者:王娇[1] 孙佳 赵来刚[1] 李瑾[1] 陆苑 李琴芬[1]
机构地区:[1]贵州医科大学附属医院,贵阳550004 [2]贵州省药物制剂重点实验室,贵阳550004
出 处:《中国药学杂志》2017年第1期57-62,共6页Chinese Pharmaceutical Journal
基 金:贵阳市科技计划项目课题(筑科合同[20111103]19号)
摘 要:目的建立同时测定新生儿脐带血和产妇外周静脉血中罗哌卡因和舒芬太尼的超高效液相串联质谱法(UPLC-MS/MS)分析方法。方法血浆样品以布比卡因为内标,采用乙酸乙酯与乙醚(1:1,V/V)进行液-液萃取。采用Waters BEH C_(18)柱(2.1mm×50mm,1.7μm)色谱柱,以0.1%甲酸乙腈-0.1%甲酸水进行梯度洗脱,流速为0.35 mL·min^(-1),柱温为45℃;质谱条件采用ESI离子源,检测方式为正离子源,多反应离子监测模式(MRM),用于定量分析的离子反应分别为m/z 275.2→m/z126.0(罗哌卡因),m/z 387.1→m/z 238.1(舒芬太尼)。结果罗哌卡因和舒芬太尼分别在0.25~202.0 ng·mL^(-1)、0.165~133.6 ng·mL^(-1)内线性关系良好(r^2>0.995)。罗哌卡因的高、中、低浓度(202、50.5、2.5 ng·mL^(-1))样本方法的平均回收率在78.46%以上,日内、日间精密度均小于8.04%。舒芬太尼的高、中、低浓度(133.6、33.4、1.65 ng·mL^(-1))样本方法的平均回收率在71.62%以上,日内、日间精密度均小于13.86%。结论所建立的分析方法简单、快速、准确、灵敏可用于临床上监测舒芬太尼和罗哌卡因的血药浓度。OBJECTIVE To establish a UPLC-MS/MS method for the determination of ropivacaine and sufentanil plasma concentration in neonate and maternal. METHODS Ropivacaine and sufentanil were extracted from plasma by ethyl acetate and ethyl ether ( 1 : 1, V/V) , and determined by LC-MS/MS using bupivacaine as the internal standard. Separation was carried on Waters BEH C18 column (2. 1 mm ×50 mm, 1.7 μm) with a mobile phase of 0. 1% formic acid acetonitrile -0. 1% formic acid water. The flow rate was 0. 35 mL . min-1 and column temperature was maitained at 45 ℃. ESI source was applied and operated in positive ion mode. Quantitative determination was performed using multiple reaction monitoring (MRM) of m/z 275. 2→m/z 126. 0 for ropivacaine, and rn/z 387. 1→m/z 238.1 for sufentanil. RESULTS There were good linearity of ropivacaine (0. 25 - 202. 0 ng . mL-1 ) and sufentanil (0. 165 - 133.6 ng . mL -1 ), and the correlation coefficient ( r2 ) were greater than 0. 995. The extraction recovery for ropivacaine and sufentanil were more than 71.62% , while the intra-day precision (RSD) were lower than 13.86%. CONCLUSION The method is accurate and high sensitive, providing a good analysis mean for monitoring neonate and maternal blood concentration of ropivacaine and sufentanil.
关 键 词:超高效液相串联质谱法 罗哌卡因 舒芬太尼 分娩镇痛 血药浓度
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