中国当代医药
中國噹代醫藥
중국당대의약
PERSON
2015年
23期
7-10
,共4页
硫酸长春地辛%顶空-气相色谱法%残留溶剂
硫痠長春地辛%頂空-氣相色譜法%殘留溶劑
류산장춘지신%정공-기상색보법%잔류용제
Vindesine sulfate%Headspace gas chromatography%Residual solvents
目的：建立顶空-气相色谱法测定硫酸长春地辛中残留溶剂甲醇、乙醇、丙酮、二氯甲烷、三氯甲烷、四氢呋喃含量的方法。方法采用聚乙二醇毛细管柱(DB-WAX),以FID为检测器,柱初始温度45℃保持10 min后升温至220℃,载气为氮气,流速为1.0 ml/min。结果甲醇在60~360μg/ml范围内,线性关系良好(r=0.9997),平均回收率为98.00%,RSD为1.30%；乙醇在100~600μg/ml范围内,线性关系良好(r=0.9997),平均回收率为99.44%,RSD为1.67%；丙酮在100~600μg/ml范围内,线性关系良好(r=0.9999),平均回收率为97.31%,R SD为2.23%；二氯甲烷在12~72μg/ml范围内,线性关系良好(r=0.9989),平均回收率为97.05%,RSD为2.59%；三氯甲烷在1~8μg/ml范围内,线性关系良好(r=0.9978),平均回收率为99.17%,RSD为4.62%；四氢呋喃在15~90μg/ml浓度范围内,浓度与峰面积呈现良好的线性关系(r=0.9998),平均回收率为95.19%,RSD为2.00%。结论本法简便,准确度好,灵敏度高,可用于硫酸长春地辛中残留溶剂的含量测定。
目的：建立頂空-氣相色譜法測定硫痠長春地辛中殘留溶劑甲醇、乙醇、丙酮、二氯甲烷、三氯甲烷、四氫呋喃含量的方法。方法採用聚乙二醇毛細管柱(DB-WAX),以FID為檢測器,柱初始溫度45℃保持10 min後升溫至220℃,載氣為氮氣,流速為1.0 ml/min。結果甲醇在60~360μg/ml範圍內,線性關繫良好(r=0.9997),平均迴收率為98.00%,RSD為1.30%；乙醇在100~600μg/ml範圍內,線性關繫良好(r=0.9997),平均迴收率為99.44%,RSD為1.67%；丙酮在100~600μg/ml範圍內,線性關繫良好(r=0.9999),平均迴收率為97.31%,R SD為2.23%；二氯甲烷在12~72μg/ml範圍內,線性關繫良好(r=0.9989),平均迴收率為97.05%,RSD為2.59%；三氯甲烷在1~8μg/ml範圍內,線性關繫良好(r=0.9978),平均迴收率為99.17%,RSD為4.62%；四氫呋喃在15~90μg/ml濃度範圍內,濃度與峰麵積呈現良好的線性關繫(r=0.9998),平均迴收率為95.19%,RSD為2.00%。結論本法簡便,準確度好,靈敏度高,可用于硫痠長春地辛中殘留溶劑的含量測定。
목적：건립정공-기상색보법측정류산장춘지신중잔류용제갑순、을순、병동、이록갑완、삼록갑완、사경부남함량적방법。방법채용취을이순모세관주(DB-WAX),이FID위검측기,주초시온도45℃보지10 min후승온지220℃,재기위담기,류속위1.0 ml/min。결과갑순재60~360μg/ml범위내,선성관계량호(r=0.9997),평균회수솔위98.00%,RSD위1.30%；을순재100~600μg/ml범위내,선성관계량호(r=0.9997),평균회수솔위99.44%,RSD위1.67%；병동재100~600μg/ml범위내,선성관계량호(r=0.9999),평균회수솔위97.31%,R SD위2.23%；이록갑완재12~72μg/ml범위내,선성관계량호(r=0.9989),평균회수솔위97.05%,RSD위2.59%；삼록갑완재1~8μg/ml범위내,선성관계량호(r=0.9978),평균회수솔위99.17%,RSD위4.62%；사경부남재15~90μg/ml농도범위내,농도여봉면적정현량호적선성관계(r=0.9998),평균회수솔위95.19%,RSD위2.00%。결론본법간편,준학도호,령민도고,가용우류산장춘지신중잔류용제적함량측정。
Objective To establish the method of headspace gas chromatography determinating the residual solvents content in vindesine sulfate such as methanol,ethanol,acetone,methylene chloride,chloroform,tetrahydrofuran. Methods Polyethylene glycol capillary column (DB-WAX) was used and FID was used as detector.The column temperature was en-hanced to 220℃after keeping the column initial temperature at 45℃for 10min.Nitrogen was used as carrier gas and its flow velocity was 1.0 ml/min. Results The linear relationship was good in the range from 60μg/ml to 360μg/ml (r=0.9997), average recovery rate was 98.00%and RSD was 1.30%.The linear relationship was good in the range from 100μg/ml to 600 μg/ml for ethanol (r=0.9997),average recovery rate was 99.44% and RSD was 1.67%.The linear relationship was good in the range from 100μg/ml to 600μg/ml for acetone (r=0.9999),average recovery rate was 97.31% and RSD was 2.23%.The linear relationship was good in the range from 12μg/ml to 72μg/ml for methylene chloride (r=0.9989),aver-age recovery rate was 97.05%and RSD was 2.59%.The linear relationship was good in the range from 1μg/ml to 8μg/ml for chloroform(r=0.9978),average recovery rate was 99.17% and RSD was 4.62%.The linear relationship was good in the range from 15 μg/ml to 90μg/ml (r=0.9998),average recovery rate was 95.19% and RSD was 2.00%. Conclusion This method is simple and has good accuracy and high sensitivity,which can be used for determination the residual solvents content in vindesine sulfate.
