山东化工
山東化工
산동화공
SHANDONG CHEMICAL INDUSTRY
2014年
7期
77-79
,共3页
毛细管气相色谱法%顶空进样%有机溶剂残留%环孢素
毛細管氣相色譜法%頂空進樣%有機溶劑殘留%環孢素
모세관기상색보법%정공진양%유궤용제잔류%배포소
capillary GC%headspace injection%residual organic solvents%cyclosporine
建立环孢素中乙醇、丙酮、乙酸乙酯的测定方法。使用配置顶空进样的气相色谱仪，用 HP -1毛细管色谱柱（100％二甲基聚硅氧烷），0.53 mm ×30 m；柱温40℃，保持5 min，以10℃·min -1的速度升温至150℃，保持2 min；以氮气为载气，流速30 cm/ min；氢火焰离子化检测器。乙醇、丙酮、乙酸乙酯线性关系良好，相关系数均大于0.99；平均回收率分别为97.75％、97.91％、98.31％；检测限分别为8.1691×10-4、3.8152×10-4、1.0082×10-7 mg/ mL。该方法的简单方便，灵敏度高，重复性好，结果准确，适用于环孢素中多种有机溶剂残留量的测定与控制。
建立環孢素中乙醇、丙酮、乙痠乙酯的測定方法。使用配置頂空進樣的氣相色譜儀，用 HP -1毛細管色譜柱（100％二甲基聚硅氧烷），0.53 mm ×30 m；柱溫40℃，保持5 min，以10℃·min -1的速度升溫至150℃，保持2 min；以氮氣為載氣，流速30 cm/ min；氫火燄離子化檢測器。乙醇、丙酮、乙痠乙酯線性關繫良好，相關繫數均大于0.99；平均迴收率分彆為97.75％、97.91％、98.31％；檢測限分彆為8.1691×10-4、3.8152×10-4、1.0082×10-7 mg/ mL。該方法的簡單方便，靈敏度高，重複性好，結果準確，適用于環孢素中多種有機溶劑殘留量的測定與控製。
건립배포소중을순、병동、을산을지적측정방법。사용배치정공진양적기상색보의，용 HP -1모세관색보주（100％이갑기취규양완），0.53 mm ×30 m；주온40℃，보지5 min，이10℃·min -1적속도승온지150℃，보지2 min；이담기위재기，류속30 cm/ min；경화염리자화검측기。을순、병동、을산을지선성관계량호，상관계수균대우0.99；평균회수솔분별위97.75％、97.91％、98.31％；검측한분별위8.1691×10-4、3.8152×10-4、1.0082×10-7 mg/ mL。해방법적간단방편，령민도고，중복성호，결과준학，괄용우배포소중다충유궤용제잔류량적측정여공제。
To establish a GC method for the determination of ethanol,acetone,ethyl acetate in cyclosporine . The GC was quipped with a headspace injector and a flame - ionization detector. A. 0. 53mm 30m,HP - 1 capillary chromatographic column(coated with 100% dimethyl polysiloxane stationary phase)was adopted and the carrier gas was nitrogen. The initial column temperature was kept at 40℃ for 5min,then raised to 150℃ at the rate of 10℃ / min - 1 ,and kept at 150℃ for 2min. The correlation coefficient in ethanol ,acetone ,ethyl acetate were all higher than 0. 99,The recovery were 97. 75% 、97. 91% 、98. 31% ;and limit of detection respectively were8. 1691 × 10 - 4、3. 8152 × 10 - 4 、1. 0082 × 10 - 7 mg/mL. This method is reliable in terms of precision,accuracy,specificity,detectability,linearity and durability. It is applicable to the detection of residual organic solvents in cyclosporine.
