首都医药
首都醫藥
수도의약
CAPITAL MEDICINE
2013年
12期
58-59
,共2页
何秀峰%刘冬%夏鹏飞%沈珑瑛%赵立敏Δ
何秀峰%劉鼕%夏鵬飛%瀋瓏瑛%趙立敏Δ
하수봉%류동%하붕비%침롱영%조립민Δ
顶空气相色谱法%水杨酸甲酯乳糖苷%残留溶剂测定
頂空氣相色譜法%水楊痠甲酯乳糖苷%殘留溶劑測定
정공기상색보법%수양산갑지유당감%잔류용제측정
Head-space Gas Chromato graphy%MSG%Determination of Residual Solvents
目的建立了测定水杨酸甲酯乳糖苷中甲醇、乙醇、二氯甲烷、乙酸乙酯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90℃,预热时间为30min,进样口温度为250℃,检测器温度为250℃,以氦气为载气,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、二氯甲烷及乙酸乙酯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、乙酸乙酯的最小检测限分别为0.35μg/mL、0.61μg/mL、0.52μg/mL、0.54μg/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,可适用于水杨酸甲酯乳糖苷中甲醇、乙醇、二氯甲烷及乙酸乙酯残留有机溶剂的测定。
目的建立瞭測定水楊痠甲酯乳糖苷中甲醇、乙醇、二氯甲烷、乙痠乙酯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90℃,預熱時間為30min,進樣口溫度為250℃,檢測器溫度為250℃,以氦氣為載氣,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、二氯甲烷及乙痠乙酯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、乙痠乙酯的最小檢測限分彆為0.35μg/mL、0.61μg/mL、0.52μg/mL、0.54μg/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,可適用于水楊痠甲酯乳糖苷中甲醇、乙醇、二氯甲烷及乙痠乙酯殘留有機溶劑的測定。
목적건립료측정수양산갑지유당감중갑순、을순、이록갑완、을산을지유궤용제함량적정공기상색보법。방법채용정공기상색보법,FID검측기,이이갑기아풍위용매,정공예열온도위90℃,예열시간위30min,진양구온도위250℃,검측기온도위250℃,이양기위재기,사용DB-624교련모세관주(30m×0.53mm, i.d,3μm),채용정서승온,실현료각조분적기선분리。결과갑순、을순、이록갑완급을산을지재각자대응적농도범위내,선성관계량호;갑순、을순、이록갑완、을산을지적최소검측한분별위0.35μg/mL、0.61μg/mL、0.52μg/mL、0.54μg/mL;가양회수솔균재95%이상,정밀도량호。결론경방법학험증,해방법령민、준학、가고,가괄용우수양산갑지유당감중갑순、을순、이록갑완급을산을지잔류유궤용제적측정。
Objective This paper reports a Head-space GC method for determination of methanol,enthanol,dichloromethane,ethylac etate in MSG.Method The analytical column was DB-624(30m×0.53mm,i.d,3μm). The injector temperature was 250℃ and the detector temperature was 250℃.The column temperature was programmed raised. The carrier gas was helium and the solvent was dimethyl sulfoxide.Results The stand curve was linear for each solvent 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 MSG.