中国药师
中國藥師
중국약사
CHINA PHARMACIST
2015年
5期
873-875,876
,共4页
毛细管气相色谱法%酒石酸托特罗定%残留有机溶剂
毛細管氣相色譜法%酒石痠託特囉定%殘留有機溶劑
모세관기상색보법%주석산탁특라정%잔류유궤용제
Capillary GC%Tolterodine tartrate%Residual organic solvent
目的：：建立毛细管气相色谱法测定酒石酸托特罗定中8种有机溶剂残留量的方法。方法：采用CP-sil 5CB色谱柱(60.0 m ×0.32 mm,5μm)；进样口温度为200℃；FID检测器温度为250℃；载气流速为1.2 ml·min-1；柱温120℃；顶空瓶平衡温度85℃,时间30 min,以二甲基甲酰胺-水(1∶4)混合溶液为溶解介质,测定酒石酸托特罗定中甲醇,乙醇,乙腈,丙酮,乙酸乙酯,三氯甲烷和四氢呋喃的残留量；采用HP-1色谱柱(30.0 m ×0.53 mm,5μm),进样口温度为220℃；FID检测器温度为250℃；载气流速为3.0 ml·min-1；柱温80℃；顶空瓶平衡温度85℃,时间30 min,以二甲亚砜-氢氧化钠溶液(17∶13)混合溶液为溶解介质,测定酒石酸托特罗定中吡啶的残留量。结果：在各色谱条件下,被测溶剂峰之间均分离良好,8种溶剂的标准曲线线性良好,相关系数均大于0.999；平均回收率为86.0%~100.2%,RSD为1.7%~3.5%(n=9)；甲醇,乙醇,乙腈,丙酮,乙酸乙酯,三氯甲烷,四氢呋喃和吡啶的检测限分别为0.63,0.43,0.30,0.18,0.079,0.36,0.18,0.89μg·ml-1。结论：该法适用于酒石酸托特罗定中这8种有机溶剂残留量的测定。
目的：：建立毛細管氣相色譜法測定酒石痠託特囉定中8種有機溶劑殘留量的方法。方法：採用CP-sil 5CB色譜柱(60.0 m ×0.32 mm,5μm)；進樣口溫度為200℃；FID檢測器溫度為250℃；載氣流速為1.2 ml·min-1；柱溫120℃；頂空瓶平衡溫度85℃,時間30 min,以二甲基甲酰胺-水(1∶4)混閤溶液為溶解介質,測定酒石痠託特囉定中甲醇,乙醇,乙腈,丙酮,乙痠乙酯,三氯甲烷和四氫呋喃的殘留量；採用HP-1色譜柱(30.0 m ×0.53 mm,5μm),進樣口溫度為220℃；FID檢測器溫度為250℃；載氣流速為3.0 ml·min-1；柱溫80℃；頂空瓶平衡溫度85℃,時間30 min,以二甲亞砜-氫氧化鈉溶液(17∶13)混閤溶液為溶解介質,測定酒石痠託特囉定中吡啶的殘留量。結果：在各色譜條件下,被測溶劑峰之間均分離良好,8種溶劑的標準麯線線性良好,相關繫數均大于0.999；平均迴收率為86.0%~100.2%,RSD為1.7%~3.5%(n=9)；甲醇,乙醇,乙腈,丙酮,乙痠乙酯,三氯甲烷,四氫呋喃和吡啶的檢測限分彆為0.63,0.43,0.30,0.18,0.079,0.36,0.18,0.89μg·ml-1。結論：該法適用于酒石痠託特囉定中這8種有機溶劑殘留量的測定。
목적：：건립모세관기상색보법측정주석산탁특라정중8충유궤용제잔류량적방법。방법：채용CP-sil 5CB색보주(60.0 m ×0.32 mm,5μm)；진양구온도위200℃；FID검측기온도위250℃；재기류속위1.2 ml·min-1；주온120℃；정공병평형온도85℃,시간30 min,이이갑기갑선알-수(1∶4)혼합용액위용해개질,측정주석산탁특라정중갑순,을순,을정,병동,을산을지,삼록갑완화사경부남적잔류량；채용HP-1색보주(30.0 m ×0.53 mm,5μm),진양구온도위220℃；FID검측기온도위250℃；재기류속위3.0 ml·min-1；주온80℃；정공병평형온도85℃,시간30 min,이이갑아풍-경양화납용액(17∶13)혼합용액위용해개질,측정주석산탁특라정중필정적잔류량。결과：재각색보조건하,피측용제봉지간균분리량호,8충용제적표준곡선선성량호,상관계수균대우0.999；평균회수솔위86.0%~100.2%,RSD위1.7%~3.5%(n=9)；갑순,을순,을정,병동,을산을지,삼록갑완,사경부남화필정적검측한분별위0.63,0.43,0.30,0.18,0.079,0.36,0.18,0.89μg·ml-1。결론：해법괄용우주석산탁특라정중저8충유궤용제잔류량적측정。
Objective:To establish a method for the determination of 8 residual organic solvents in tolterodine tartrate by capillary GC. Methods: The determination of methanol, ethanol, acetonitrile, acetone, ethyl acetate, trichloromethane and tetrahydrofuran in tolterodine tartrate dissolved in the solution of N, N-dimethylformamide-water ( 1∶ 4 ) was carried out on a CP-sil 5CB ( 60. 0 m × 0. 32 mm,5μm)column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The flow rate of carrier gas was 1. 2 ml·min-1 . The column temperature was 120℃. The headspace vial temperature was 85℃ and the time was 30min. The determina-tion of pyridine in tolterodine tartrate dissolved in the solution of dimethylsulfoxide-sodium hydroxide (17∶13) was carried out on an HP-1(30. 0 m × 0. 53 mm,5 μm) column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column tem-perature was 80℃. The flow rate of carrier gas was 3. 0 ml·min-1 . The headspace vial temperature was 85℃ and the time was 30 min. Results:All peaks could be separated from each other under the chromatographic conditions. The linearity of the eight solvents was falrly good (r>0. 999). The average recovery was ranged from 86. 0% to 100. 2% with RSD of 1. 7%-3. 5% (n=9). The limit of detection was 0. 63, 0. 43, 0. 30, 0. 18, 0. 079, 0. 36, 0. 18 and 0. 89 μg·ml-1 , respectively. Conclusion:The methods can be applied in the determination of the eight residual organic solvents in tolterodine tartrate.
