毛细管气相色谱法测定注射用地西他滨中的残留溶剂

目的:建立测定注射用地西他滨中残留溶剂的方法。方法:采用毛细管气相色谱法,按内标法计算残留溶剂的含量。色谱柱为Agilent DB-624毛细管柱,检测器为氢火焰离子化检测器,检测器温度为280℃,进样口温度为230℃,柱温采用程序升温,载气为高纯氮,流速为1.5 ml/min,分流比为50∶1,进样方式为直接进样,进样量为1μl。结果:乙醇、乙醚、异丙醇、乙腈、二氯甲烷、四氢呋喃、环己烷、甲苯、N,N-二甲基甲酰胺的检测质量浓度线性范围分别为0.100 3~2.507、0.101 3~2.532、0.102 2~2.556、0.008 3~0.207 8、0.012 4~0.309 3、0.014 8~0.369 4、0.078 1~1.953、0.024 9~1.250、0.017 6~0.440 9 mg/ml(r均≥0.999 2);精密度、重复性试验的RSD<2%;加样回收率为96.70%~101.60%,RSD为0.59%~1.82%(n=9)。结论:该方法简便、准确、重复性好,适用于注射用地西他滨中残留溶剂的测定。     

毛细管气相色谱法检测头孢西丁钠原料药中的残留溶剂

目的 建立气相色谱法测定头孢西丁钠原料药中的有机残留溶剂乙醇、丙酮及乙酸乙酯.方法 色谱柱为HP-5(30m×0.53mm×1.5μm),载气为氮气,进样器温度为180℃,火焰离子检测器(FID)温度为250℃,柱温为50℃,以水为溶剂,进样量1μl.结果 乙醇、丙酮及乙酸乙酯的线性关系r分别为0.9998、0.999及0.997,平均回收率分别为98.6%、102.6%及101.9%,最小检出量分别为6.0E～4ng、2.9E～4ng及3.1E～4ng.3批样品中均检测出丙酮残留,而未检出乙醇和乙酸乙酯.结论 该方法 高效、灵敏、准确,适用于同时检测头孢西丁钠原料药中有机残留溶剂乙醇、丙酮及乙酸乙酯的含量.     

毛细管气相色谱法检测头孢西丁钠原料药中的残留溶剂

目的建立气相色谱法测定头孢西丁钠原料药中的有机残留溶剂乙醇、丙酮及乙酸乙酯。方法色谱柱为HP-5(30m×0.53mm×1.5μm),载气为氮气,进样器温度为180℃,火焰离子检测器(FID)温度为250℃,柱温为50℃,以水为溶剂,进样量1μl。结果乙醇、丙酮及乙酸乙酯的线性关系r分别为0.9998、0.999及0.997,平均回收率分别为98.6%、102.6%及101.9%,最小检出量分别为6.0E～4ng、2.9E～4ng及3.1E～4ng。3批样品中均检测出丙酮残留,而未检出乙醇和乙酸乙酯。结论该方法高效、灵敏、准确,适用于同时检测头孢西丁钠原料药中有机残留溶剂乙醇、丙酮及乙酸乙酯的含量。     

毛细管气相色谱法检测葛根素衍生物中的残留溶剂

目的:建立葛根素衍生物中二氯甲烷、丙酮、乙酸乙酯、吡啶4种有机溶剂残留量的检测方法。方法:采用气相色谱法,色谱柱为 HP-5(交联5%苯甲基聚硅氧烷)毛细管柱(30m×0.53mm×0.23μm),载气为氮气。检测器温度:250℃;进样口温度:280℃;程序升温:初始温度为36℃,保持0.5min,以每分钟3℃升至70℃,保持1min(延迟时间3min,保持250℃)。分流进样,分流比为1:100,柱前压为37.5kPa。结果:被测物均得到很好的分离,峰面积与浓度呈现良好的线性关系,精密度良好。结论:本方法简单、快捷,且灵敏度高,可用于葛根素衍生物中的残留溶剂检测。     

毛细管气相色谱法检测右丙亚胺中的残留溶剂

目的:建立毛细管气相色谱法定量检测右丙亚胺原料药中的残留溶剂.方法:色谱柱为OV-101(30 m×0.53 mm,1 μm),柱温采用程序升温,载气为氮气,采用氢离子火焰检测器;以1,2-二氯乙烷为内标,测定右丙亚胺中的有机残留溶剂为甲醇、二氧六环、N,N-二甲基甲酰胺.结果:在本色谱条件下,测得各组分的线性关系良好(r均在0.996 5以上);平均回收率分别为100.1%、99.8%、99.0%;最低检测限分别为0.1024、0.199、0.448 μg·mL-1.结论:方法灵敏,准确,适用于右丙亚胺中残留溶剂的检测.     

高效液相色谱法测定氯法拉滨注射液中氯法拉滨的含量

目的:建立高效液相色谱法测定氯法拉滨注射液中主药氯法拉滨的含量.方法:采用Shim-pack VP-ODS(5 μm,4.6 mm ×150 mm)色谱柱,流动相为乙腈·乙酸铵溶液(取乙酸铵0.31 g,加水溶解并稀释至1000 mL,再加甲酸1.0 mE)(10:90),流速1.0 mL/min,进样量20μL,检测波长262 nm.结果:氯法拉滨在进样量0.4～242.5μg/mL范围内线性关系良好,回归方程为A=23156C+12378(r=0.9999,n=5),平均加样回收率为99.97%,RSD为0.40%.结论:本方法快速、简便、结果准确,可用于控制该制剂的质量.     

毛细管气相色谱法测定罗红霉素中的残留溶剂

［摘要］目的建立顶空进样和直接进样毛细管气相色谱方法测定罗红霉素中的残留溶剂。方法甲醇、丙酮测定采用顶空进样法,色谱柱为DB 624（6%氰丙基苯基 94%二甲基聚硅氧烷固定液）石英毛细管柱（30.0 m×0.53 mm,3.0 μm）,柱温40 ℃维持5 min,以每分钟 30 ℃速率升至200 ℃,维持3 min,溶剂为二甲亚砜;醋酸、二甲基甲酰胺测定采用直接进样法,色谱柱为DB 624石英毛细管柱（30.0 m×0.53 mm,3.0 μm）,柱温100 ℃维持6 min,以每分钟30 ℃速率升至200 ℃,维持5 min,溶剂为二甲亚砜。结果被测物均能得到很好分离,峰面积与浓度呈良好的线性关系,精密度和回收率良好。结论该方法可用于罗红霉素原料药中残留溶剂的检测。     

GC法检测氯法拉滨中有机溶剂的残留量

目的:建立以气相色谱法检测氯法拉滨原料药中7种有机溶剂残留量的方法。方法:毛细管柱为AT-1301;载气为氮气;检测器为火焰离子化检测器;柱温采取程序升温,初始温度40℃,以7℃.min-1升至80℃,再以20℃.min-1升至200℃,保持2min;进样口温度250℃;检测器温度280℃;分流直接进样。检测3批氯法拉滨原料药中甲醇、乙腈、二氯甲烷、叔丁醇、乙酸乙酯、正庚烷、乙酸的残留量。结果:各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好(r=0.99941～0.99993),平均回收率为96.5%～102.4%,RSD均小于4.0%,3批样品中7种有机溶剂残留量均符合《中国药典》要求。结论:本方法灵敏、准确、可靠,可用于氯法拉滨原料药中有机溶剂残留量的检测。     

毛细管气相色谱法测定西布曲明中有机溶剂残留量

目的建立西布曲明中有机溶剂残留量的测定方法.方法采用毛细管气相色谱法,使用HP-INNOWAX色谱柱(30 m×0.53 mm,2.65 μm),程序升温技术,标准对照法分离测定西布曲明中的残留有机溶剂.结果 3批样品中的有机溶剂残留量均符合要求.建立的色谱方法对待测溶剂具有良好的分离度,在所考察的浓度范围内线性关系良好,各回收率均得到满意结果.结论该方法灵敏、准确,适用于西布曲明中有机溶剂残留量的测定.     

毛细管气相色谱法测定替米沙坦有机溶剂残留量

目的建立气相色谱法分别测定替米沙坦中残留有机溶剂甲醇、乙醇、丙酮、二氯甲烷、氯仿、乙二醇和二甲基甲酰胺。方法以DB624弹性石英毛细管柱为色谱柱（30m&#215;0．53mm）．载气为氮气,采用氢火焰离子化检测器,进样1：2温度为200℃,检测器温度为250℃。顶空进样法采用程序升温（50℃,保持15min。以30℃&#183;min^-1升至160℃,保持5min）,进样量1．0mL。直接进样法柱温为100℃．进样量1．0μL。结果3批样品中7种有机溶剂残留量均符合规定。结论本方法可测定替米沙坦中的有机溶剂残留量,方法简单准确。     

气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量

目的建立盐酸洛哌丁胺中4种有机溶剂残留量的分离测定方法。方法采用毛细管气相色谱法,FID检测器,在毛细管色谱柱J＆WDB-624上程序升温,载气为氮气,进样口温度200℃,检测器温度250℃,测定盐酸洛哌丁胺中异丙醇、乙酸乙酯、甲基异丁基酮、甲苯的残留量。结果待测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论本实验建立的方法灵敏、准确,适用于盐酸洛哌丁胺中有机溶剂残留量的检测。     

气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量

Objective To investigate a method of detecting four residual solvents in loperamide hydrochlo-fide. Methods The residual solvents in ioperamide hydrochloride included isopropanol, ethyl acetate, Methyl isobutyl ketone and methylbenzene. The concetrations were quantitatively detemined by headspace GC on J&W DB-624 column, FID detector. Nitrogen was used as the carry gas. The injector temperature was 200% and the detector temperature was 25℃, meanwhile the column temperature was programmed raised. Results The solvents were completely separated and the calibration CHives of each solvent showed good linear relationship within a certain range. Conclusion The method is sensitive, accurate and can be used for quality control.     

气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量

Objective To investigate a method of detecting four residual solvents in loperamide hydrochlo-fide. Methods The residual solvents in ioperamide hydrochloride included isopropanol, ethyl acetate, Methyl isobutyl ketone and methylbenzene. The concetrations were quantitatively detemined by headspace GC on J&W DB-624 column, FID detector. Nitrogen was used as the carry gas. The injector temperature was 200% and the detector temperature was 25℃, meanwhile the column temperature was programmed raised. Results The solvents were completely separated and the calibration CHives of each solvent showed good linear relationship within a certain range. Conclusion The method is sensitive, accurate and can be used for quality control.     

气相色谱法测定米格列奈钙中6种有机溶剂残留量

目的：建立米格列奈钙中6种有机溶剂残留量的分离测定方法。方法：采用顶空进样毛细管气相色谱法，FID检测器，色谱柱为HP-INNO Wax毛细管柱，载气为氮气，柱温30℃，测定了米格列奈钙原料中乙醚、四氢呋喃、乙酸乙酯、甲醇、二氯甲烷和乙醇的残留量。结果：6种有机溶剂完全分离，在所考察范围内线性关系良好，加样回收率均得到满意结果。结论：本实验建立的方法灵敏、准确，适用于米格列奈钙中有机溶剂残留量的检测。     

气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量

Objective To investigate a method of detecting four residual solvents in loperamide hydrochlo-fide. Methods The residual solvents in ioperamide hydrochloride included isopropanol, ethyl acetate, Methyl isobutyl ketone and methylbenzene. The concetrations were quantitatively detemined by headspace GC on J&W DB-624 column, FID detector. Nitrogen was used as the carry gas. The injector temperature was 200% and the detector temperature was 25℃, meanwhile the column temperature was programmed raised. Results The solvents were completely separated and the calibration CHives of each solvent showed good linear relationship within a certain range. Conclusion The method is sensitive, accurate and can be used for quality control.     

气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量

Objective To investigate a method of detecting four residual solvents in loperamide hydrochlo-fide. Methods The residual solvents in ioperamide hydrochloride included isopropanol, ethyl acetate, Methyl isobutyl ketone and methylbenzene. The concetrations were quantitatively detemined by headspace GC on J&W DB-624 column, FID detector. Nitrogen was used as the carry gas. The injector temperature was 200% and the detector temperature was 25℃, meanwhile the column temperature was programmed raised. Results The solvents were completely separated and the calibration CHives of each solvent showed good linear relationship within a certain range. Conclusion The method is sensitive, accurate and can be used for quality control.