中华麻醉学杂志
中華痳醉學雜誌
중화마취학잡지
CHINESE JOURNAL OF ANESTHESIOLOGY
2013年
12期
1464-1467
,共4页
气相色谱-质谱法%舒芬太尼%血药浓度
氣相色譜-質譜法%舒芬太尼%血藥濃度
기상색보-질보법%서분태니%혈약농도
Gas chromatography-mass spectrometry%Sufentanil%Plasma concentration
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.
目的 對氣相色譜-質譜法(GC-MS法)測定血漿舒芬太尼濃度進行改良.方法 以芬太尼為內標,血漿標本經乙痠乙酯-石油醚萃取,採用色譜柱HP-5MS,初始溫度為130℃,最終溫度為320℃,進樣口溫度為290℃,接口溫度為300℃.載氣為高純氦氣(純度99.999％),恆流流速為1ml/min,進樣方式為不分流進樣,進樣體積為1μl.質譜條件中選用EI源,離子源溫度230℃,四級桿溫度150℃,電子轟擊能量70 eV,倍增電壓2112 V,選擇性離子鑑測模式.溶劑延遲為7 min,分組進行採集,根據舒芬太尼及芬太尼的離子特徵麯線于8.20～8.40 min採集舒芬太尼的特徵離子,7.60～7.80 min採集芬太尼特徵離子.結果 標準麯線提示舒芬太尼濃度在0.02～ 10.00 ng/ml範圍內與色譜條件下的峰麵積比線性關繫良好,其方程:y=0.1625X+ 0.0316,R2=0.9987,萃取迴收率＞80％,日內和日間精密度均小于8％,最低檢測濃度為0.02 ng/ml.結論 GC-MS改良法測定舒芬太尼血藥濃度,不僅測定敏感、準確,而且操作簡化,更適用于舒芬太尼的藥理學研究.
목적 대기상색보-질보법(GC-MS법)측정혈장서분태니농도진행개량.방법 이분태니위내표,혈장표본경을산을지-석유미췌취,채용색보주HP-5MS,초시온도위130℃,최종온도위320℃,진양구온도위290℃,접구온도위300℃.재기위고순양기(순도99.999％),항류류속위1ml/min,진양방식위불분류진양,진양체적위1μl.질보조건중선용EI원,리자원온도230℃,사급간온도150℃,전자굉격능량70 eV,배증전압2112 V,선택성리자감측모식.용제연지위7 min,분조진행채집,근거서분태니급분태니적리자특정곡선우8.20～8.40 min채집서분태니적특정리자,7.60～7.80 min채집분태니특정리자.결과 표준곡선제시서분태니농도재0.02～ 10.00 ng/ml범위내여색보조건하적봉면적비선성관계량호,기방정:y=0.1625X+ 0.0316,R2=0.9987,췌취회수솔＞80％,일내화일간정밀도균소우8％,최저검측농도위0.02 ng/ml.결론 GC-MS개량법측정서분태니혈약농도,불부측정민감、준학,이차조작간화,경괄용우서분태니적약이학연구.
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.
