摘要
目的 对气相色谱-质谱法（GC-MS法）测定血浆舒芬太尼浓度进行改良.方法 以芬太尼为内标,血浆标本经乙酸乙酯-石油醚萃取,采用色谱柱HP-5MS,初始温度为130℃,最终温度为320℃,进样口温度为290℃,接口温度为300℃.载气为高纯氦气（纯度99.999％）,恒流流速为1ml/min,进样方式为不分流进样,进样体积为1μl.质谱条件中选用EI源,离子源温度230℃,四级杆温度150℃,电子轰击能量70 eV,倍增电压2112 V,选择性离子监测模式.溶剂延迟为7 min,分组进行采集,根据舒芬太尼及芬太尼的离子特征曲线于8.20～8.40 min采集舒芬太尼的特征离子,7.60～7.80 min采集芬太尼特征离子.结果 标准曲线提示舒芬太尼浓度在0.02～ 10.00 ng/ml范围内与色谱条件下的峰面积比线性关系良好,其方程：y=0.1625X＋ 0.0316,R2=0.9987,萃取回收率＞80％,日内和日间精密度均小于8％,最低检测浓度为0.02 ng/ml.结论 GC-MS改良法测定舒芬太尼血药浓度,不仅测定敏感、准确,而且操作简化,更适用于舒芬太尼的药理学研究.
Objective To modify gas chromatography-mass spectrometry （GC-MS） for determination of plasma sufentanil concentrations.Methods Fentanyl was used as the internal standard.The plasma samples were extracted with ethyl acetate and petroleum ether.An HP-5MS capillary column was used.The initial temperature of the column was set at 130 ℃,and the final temperature was 320 ℃.The injector port temperature was set at 290 ℃,and the interface temperature was 300 ℃.The carrier gas was high purity helium （purity 99.999%） with a constant flow rate of 1 ml/min.The injection volume was 1 μl with splitless injection.The MS conditions were as follows：EI source,ion source temperature 230 ℃,four-pole temperature 150 ℃,electron bombardment energy 70 eV,multiply voltage 2112 V,selective ion monitoring mode,solvent delay 7 min.The characteristic ions of sufentanil and fentanyl were obtained in 8.20-8.40 min and 7.60-7.80 min,respectively,according to the characteristic ion curve of sufentanil and fentanyl.Results The standard curve of sufentanil had good linear relationship in the range of 0.02-10.00 ng/ml and the equation was Y =0.1625X ＋ 0.0316,R2 =0.9987.The extraction recovery was more than 80%,intra-day and inter-day determinations were less than 8%,and the limit of detection was 0.02 ng/ml.Conclusion When modified GC-MS is applied to determine the concentrations of sufentanil in plasma,not only the determination is sensitive and accurate,but also the procedures are simplified,and it is more suitable for the pharmacological research of sufentanil.
出处
《中华麻醉学杂志》
CAS
CSCD
北大核心
2013年第12期1464-1467,共4页
Chinese Journal of Anesthesiology
关键词
气相色谱-质谱法
舒芬太尼
血药浓度
Gas chromatography-mass spectrometry
Sufentanil
Plasma concentration
