中国药师
中國藥師
중국약사
CHINA PHARMACIST
2015年
6期
888-889,925
,共3页
溴芬酸钠%有机溶剂残留%顶空气相色谱法
溴芬痠鈉%有機溶劑殘留%頂空氣相色譜法
추분산납%유궤용제잔류%정공기상색보법
Bromfenac sodium%Residual solvents%Headspace gas chromatography
目的：：建立顶空毛细管气相色谱法测定溴芬酸钠中有机溶剂残留量。方法：采用顶空气相色谱法,色谱柱为HP-5毛细管柱,载气为氮气,流速为0.8 ml·min-1。 FID检测器,检测器温度为250℃；进样口温度为200℃；柱温采取程序升温,初始温度40℃,维持10 min,以30℃·min-1升温至150℃,维持5 min。顶空进样,顶空瓶平衡温度为100℃,平衡时间为20 min。以二甲亚砜为溶剂,外标法测定溴芬酸钠中甲苯、异丙醇、二氯甲烷、甲醇及异丙醚的残留量。结果：各组分完全分离,线性关系良好,5种溶剂的平均回收率分别为98.9%( RSD =2.01%)、99.2%( RSD =1.95%)、99.6%( RSD =1.65%)、100.5%( RSD =1.38%)、100.8%(RSD=1.36%)(n=9)。结论：该法简便、准确,可用于溴芬酸钠中5种有机溶剂残留量的测定。
目的：：建立頂空毛細管氣相色譜法測定溴芬痠鈉中有機溶劑殘留量。方法：採用頂空氣相色譜法,色譜柱為HP-5毛細管柱,載氣為氮氣,流速為0.8 ml·min-1。 FID檢測器,檢測器溫度為250℃；進樣口溫度為200℃；柱溫採取程序升溫,初始溫度40℃,維持10 min,以30℃·min-1升溫至150℃,維持5 min。頂空進樣,頂空瓶平衡溫度為100℃,平衡時間為20 min。以二甲亞砜為溶劑,外標法測定溴芬痠鈉中甲苯、異丙醇、二氯甲烷、甲醇及異丙醚的殘留量。結果：各組分完全分離,線性關繫良好,5種溶劑的平均迴收率分彆為98.9%( RSD =2.01%)、99.2%( RSD =1.95%)、99.6%( RSD =1.65%)、100.5%( RSD =1.38%)、100.8%(RSD=1.36%)(n=9)。結論：該法簡便、準確,可用于溴芬痠鈉中5種有機溶劑殘留量的測定。
목적：：건립정공모세관기상색보법측정추분산납중유궤용제잔류량。방법：채용정공기상색보법,색보주위HP-5모세관주,재기위담기,류속위0.8 ml·min-1。 FID검측기,검측기온도위250℃；진양구온도위200℃；주온채취정서승온,초시온도40℃,유지10 min,이30℃·min-1승온지150℃,유지5 min。정공진양,정공병평형온도위100℃,평형시간위20 min。이이갑아풍위용제,외표법측정추분산납중갑분、이병순、이록갑완、갑순급이병미적잔류량。결과：각조분완전분리,선성관계량호,5충용제적평균회수솔분별위98.9%( RSD =2.01%)、99.2%( RSD =1.95%)、99.6%( RSD =1.65%)、100.5%( RSD =1.38%)、100.8%(RSD=1.36%)(n=9)。결론：해법간편、준학,가용우추분산납중5충유궤용제잔류량적측정。
Objective:To establish a headspace capillary GC method for the determination of residual solvents in bromfenac sodi-um. Methods:A headspace GC was used to separate the residual solvents on an HP-5 capillary column with an FID detector. The car-rier gas was nitrogen at the flow rate of 0. 8 ml·min-1 . The temperature of the injector was 200 ℃ and that of the FID was 250 ℃. The programmed column temperature was set as follows:maintained at 40℃ for 10 min, and then raised to 150℃ at the rate of 30℃·min-1 and maintained for 5 min. The containers of headspace injector were in equilibrium at 100 ℃ for 20 min. Dimethyl sulfoxide was used as the solvent. The amount of the residual solvents, such as methylbenzene, isopropanol, dichloromethane, methanol and iso-propyl ether was calculated by an external standard method. Results:All the solvents could be completely separated with good linear relationship. The average recovery of the five solvents was 98. 9%( RSD =2. 01%),99. 2% ( RSD =1. 95%),99. 6% ( RSD =1. 65%),100. 5%(RSD=1. 38%)and 100. 8%(RSD=1. 36%)(n=9),respectively. Conclusion:The method is simple and accu-rate in the determination of the five residual solvents in bromfenac sodium.
