首都医药
首都醫藥
수도의약
CAPITAL MEDICINE
2013年
10期
68-69
,共2页
田昕%刘思飞%赵明%韩程亮Δ
田昕%劉思飛%趙明%韓程亮Δ
전흔%류사비%조명%한정량Δ
顶空气相色谱法%格拉司琼%残留溶剂
頂空氣相色譜法%格拉司瓊%殘留溶劑
정공기상색보법%격랍사경%잔류용제
Head-Space Gas Chromatography%Granisetron%Determination of Residual Solvents
目的建立测定格拉司琼中甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃残留有机溶剂含量的顶空气相色谱法.方法采用顶空气相色谱法,FID检测器,以二甲基亚砜为溶媒,顶空预热温度为95℃,预热时间为25min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-624交联毛细管柱(30m×0.53mm.i.d,3μm),采用程序升温,实现了各组分的基线分离.结果甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃在各自对应的浓度范围内,线性关系良好;甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃的最小检测限分别为0.01μg/mL、0.19μg/mL、0.02μg/mL、0.18μg/mL、0.02μg/mL、0.003μg/mL;加样回收率均在95%以上,精密度良好.结论经方法学验证,该方法灵敏、准确、可靠,可适用于格拉司琼中甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃残留有机溶剂的测定.
目的建立測定格拉司瓊中甲醇、乙醇、二氯甲烷、異丙醇、乙痠乙酯、四氫呋喃殘留有機溶劑含量的頂空氣相色譜法.方法採用頂空氣相色譜法,FID檢測器,以二甲基亞砜為溶媒,頂空預熱溫度為95℃,預熱時間為25min,進樣口溫度為180℃,檢測器溫度為250℃,以氮氣為載氣,使用DB-624交聯毛細管柱(30m×0.53mm.i.d,3μm),採用程序升溫,實現瞭各組分的基線分離.結果甲醇、乙醇、二氯甲烷、異丙醇、乙痠乙酯、四氫呋喃在各自對應的濃度範圍內,線性關繫良好;甲醇、乙醇、二氯甲烷、異丙醇、乙痠乙酯、四氫呋喃的最小檢測限分彆為0.01μg/mL、0.19μg/mL、0.02μg/mL、0.18μg/mL、0.02μg/mL、0.003μg/mL;加樣迴收率均在95%以上,精密度良好.結論經方法學驗證,該方法靈敏、準確、可靠,可適用于格拉司瓊中甲醇、乙醇、二氯甲烷、異丙醇、乙痠乙酯、四氫呋喃殘留有機溶劑的測定.
목적건립측정격랍사경중갑순、을순、이록갑완、이병순、을산을지、사경부남잔류유궤용제함량적정공기상색보법.방법채용정공기상색보법,FID검측기,이이갑기아풍위용매,정공예열온도위95℃,예열시간위25min,진양구온도위180℃,검측기온도위250℃,이담기위재기,사용DB-624교련모세관주(30m×0.53mm.i.d,3μm),채용정서승온,실현료각조분적기선분리.결과갑순、을순、이록갑완、이병순、을산을지、사경부남재각자대응적농도범위내,선성관계량호;갑순、을순、이록갑완、이병순、을산을지、사경부남적최소검측한분별위0.01μg/mL、0.19μg/mL、0.02μg/mL、0.18μg/mL、0.02μg/mL、0.003μg/mL;가양회수솔균재95%이상,정밀도량호.결론경방법학험증,해방법령민、준학、가고,가괄용우격랍사경중갑순、을순、이록갑완、이병순、을산을지、사경부남잔류유궤용제적측정.
Objective This paper reports a Head-space GC method for determination of methanol,enthanol,2-propanol,dichlor omethane,ethylacetate,tetrahy drofuran in granisetron.Method The analytical column was DB-624(30m×0.53mm.i.d,3μm). The injector temperature was 180℃ and the detector temperature was 250℃.The column temperature was programmed raised.The carrier gas was nitrogen and the solvent was diethyl suffixed.Results The stand curve were linear for each solvents in the range of each consistency.The average recoveries were all more than 95%.Conclusion This method is simple,rapid and precise,it is suitable for measurement of residual solvents in Granisetron.