今日药学
今日藥學
금일약학
PHARMACY TODAY
2009年
7期
50-52
,共3页
顶空气相色谱法%美伐他汀%残留溶剂
頂空氣相色譜法%美伐他汀%殘留溶劑
정공기상색보법%미벌타정%잔류용제
headspace gas chromatography%Mevastatin%residue solvent
目的 建立美伐他汀中有机残留溶剂的测定方法.方法 顶空气相色谱法.色谱条件:采用HB-5(30.0 m×0.32 mm×0.25 μm)硅胶键合毛细管柱;柱温:初始温度为40℃,保持5 min后,升至90℃,升温速率为2℃/min,保持0 min,升至160℃,升温速率为30℃/min,保持2 min;检测器:火焰离子化检测器;进样器温度:220℃;检测器温度:260℃;载气:氮气;流速:4 ml/min;分流比:1:10.结果 丙酮在15.8～79.0μg/ml、乙酸乙酯在18.0～90 μg/ml、甲苯在8.7～43.3 μg/ml范围内峰面积与浓度呈较好线性关系.平均回收率(n=9)分别为丙酮101.0%,相对标准偏差值(RSD)=1.6%;乙酸乙酯99.8%,RSD=1.0%.结论 本方法操作简便、结果准确,是控制美伐他汀中残留溶剂的可靠方法.
目的 建立美伐他汀中有機殘留溶劑的測定方法.方法 頂空氣相色譜法.色譜條件:採用HB-5(30.0 m×0.32 mm×0.25 μm)硅膠鍵閤毛細管柱;柱溫:初始溫度為40℃,保持5 min後,升至90℃,升溫速率為2℃/min,保持0 min,升至160℃,升溫速率為30℃/min,保持2 min;檢測器:火燄離子化檢測器;進樣器溫度:220℃;檢測器溫度:260℃;載氣:氮氣;流速:4 ml/min;分流比:1:10.結果 丙酮在15.8～79.0μg/ml、乙痠乙酯在18.0～90 μg/ml、甲苯在8.7～43.3 μg/ml範圍內峰麵積與濃度呈較好線性關繫.平均迴收率(n=9)分彆為丙酮101.0%,相對標準偏差值(RSD)=1.6%;乙痠乙酯99.8%,RSD=1.0%.結論 本方法操作簡便、結果準確,是控製美伐他汀中殘留溶劑的可靠方法.
목적 건립미벌타정중유궤잔류용제적측정방법.방법 정공기상색보법.색보조건:채용HB-5(30.0 m×0.32 mm×0.25 μm)규효건합모세관주;주온:초시온도위40℃,보지5 min후,승지90℃,승온속솔위2℃/min,보지0 min,승지160℃,승온속솔위30℃/min,보지2 min;검측기:화염리자화검측기;진양기온도:220℃;검측기온도:260℃;재기:담기;류속:4 ml/min;분류비:1:10.결과 병동재15.8～79.0μg/ml、을산을지재18.0～90 μg/ml、갑분재8.7～43.3 μg/ml범위내봉면적여농도정교호선성관계.평균회수솔(n=9)분별위병동101.0%,상대표준편차치(RSD)=1.6%;을산을지99.8%,RSD=1.0%.결론 본방법조작간편、결과준학,시공제미벌타정중잔류용제적가고방법.
Objective To establish a method for determination of residue solvent in Mevastatin. Methods Headspace gas chromatography was used. The HB-5 capillary colunm (30.0 m×0.32 mm×0.25 μm) were used; nitrogen was used as the carry gas; the initial temperature of column was 40℃, and kept for 5 min, than turn to 90℃ by the rate of 2℃/min, and after that turn to 160℃ by the rate of 30℃/min and kept for 2 min; the injector was set at 220℃ and FID detector at 260℃; the flow rate was 4 mL/min; the distributary rate was 1: 10. Results The calibration curves for acetone, ethyl-acetate, and toluene were linear in the rang of 15. 8～79. 0 μg/ml, 18. 0～90μg/ml, and 8. 7～43.3μg/ml,respectively. The average recoveries of acetone and ethyl-acetate were 101.0% (RSD=1.6%, n=9) and 99.8% (RSD=1.0%, n=9), respectively. Conclusion This method is easy to operate with precise result, and is a reliable method for the control of residue solvent of Mevastatin.
