中国药师
中國藥師
중국약사
CHINA PHARMACIST
2014年
10期
1784-1785
,共2页
盐酸克林霉素%有机溶剂残留%顶空气相色谱法
鹽痠剋林黴素%有機溶劑殘留%頂空氣相色譜法
염산극림매소%유궤용제잔류%정공기상색보법
Clindamycinhydrochloride%Residualsolvents%Headspacegaschromatography
目的：：建立顶空毛细管气相色谱法测定盐酸克林霉素中有机溶剂残留量。方法：采用顶空气相色谱法,色谱柱为DB-624毛细管柱,载气为氮气,流速为2 ml·min-1,分流比为1∶1。 FID检测器,检测器温度为300℃；进样口温度为200℃；柱温采取程序升温,起始温度40℃,保持5 min,以20℃·min-1升温至200℃,持续10 min。顶空进样,平衡温度为80℃,平衡时间为30 min。以水为溶剂,外标法测定盐酸克林霉素中甲醇,乙醇,丙酮,三氯甲烷和N,N-二甲基甲酰胺的残留量。结果：在此色谱条件下,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=0.9991~0.9999；平均回收率为97.2%~101.2%,RSD为0.68%~1.98%(n=9)。结论：本试验建立的顶空气相色谱方法适合盐酸克林霉素原料中有机溶剂残留量的检测。
目的：：建立頂空毛細管氣相色譜法測定鹽痠剋林黴素中有機溶劑殘留量。方法：採用頂空氣相色譜法,色譜柱為DB-624毛細管柱,載氣為氮氣,流速為2 ml·min-1,分流比為1∶1。 FID檢測器,檢測器溫度為300℃；進樣口溫度為200℃；柱溫採取程序升溫,起始溫度40℃,保持5 min,以20℃·min-1升溫至200℃,持續10 min。頂空進樣,平衡溫度為80℃,平衡時間為30 min。以水為溶劑,外標法測定鹽痠剋林黴素中甲醇,乙醇,丙酮,三氯甲烷和N,N-二甲基甲酰胺的殘留量。結果：在此色譜條件下,各有機溶劑均能得到有效分離,在所攷察的濃度範圍內線性關繫良好,r=0.9991~0.9999；平均迴收率為97.2%~101.2%,RSD為0.68%~1.98%(n=9)。結論：本試驗建立的頂空氣相色譜方法適閤鹽痠剋林黴素原料中有機溶劑殘留量的檢測。
목적：：건립정공모세관기상색보법측정염산극림매소중유궤용제잔류량。방법：채용정공기상색보법,색보주위DB-624모세관주,재기위담기,류속위2 ml·min-1,분류비위1∶1。 FID검측기,검측기온도위300℃；진양구온도위200℃；주온채취정서승온,기시온도40℃,보지5 min,이20℃·min-1승온지200℃,지속10 min。정공진양,평형온도위80℃,평형시간위30 min。이수위용제,외표법측정염산극림매소중갑순,을순,병동,삼록갑완화N,N-이갑기갑선알적잔류량。결과：재차색보조건하,각유궤용제균능득도유효분리,재소고찰적농도범위내선성관계량호,r=0.9991~0.9999；평균회수솔위97.2%~101.2%,RSD위0.68%~1.98%(n=9)。결론：본시험건립적정공기상색보방법괄합염산극림매소원료중유궤용제잔류량적검측。
Objective:To establish a headspace capillary gas chromatography method for the determination of residual solvents in clindamycin hydrochloride. Methods:A headspace gas chromatography was used to separate the residual solvents on a DB-624 capillary column with an FID detector. The carried gas was nitrogen at a flow rate of 2ml·min-1 . The split ratio was 1∶1. The temperature of the injector was 200℃ and that of the FID was 300℃. The programmed column temperature was set as follows:maintained at 40℃ for 5 min and then raised to 200℃ at the rate of 20℃·min-1 and maintained for 10 min. The containers of headspace injector were in e-quilibrium at 80℃ for 30 min. Water was used as the solvent. The amounts of the residual solvents such as methanol,ethanol,acetone, chloroform and N,N-dimethyformamide were calculated by an external standard method. Results:The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship (r=0. 999 1 ~0. 999 9). The average recovery was within the range of 97. 2% ~101. 2% and RSD was within the range of 0. 68% ~1. 98%(n=9). Conclusion:The method is suit-able for the determination of residual solvents in clindamycin hydrochloride.
