中国药师
中國藥師
중국약사
CHINA PHARMACIST
2014年
9期
1588-1589,1590
,共3页
舒展%王琤帅%郑篮君%应斌斌
舒展%王琤帥%鄭籃君%應斌斌
서전%왕쟁수%정람군%응빈빈
奥沙拉秦钠%残留溶剂%顶空气相色谱法
奧沙拉秦鈉%殘留溶劑%頂空氣相色譜法
오사랍진납%잔류용제%정공기상색보법
Olsalazine sodium%Residual organic solvent%Headspace GC
目的:改进奥沙拉秦钠残留溶剂的测定方法。方法:采用气相色谱顶空进样,色谱柱为DB-624弹性毛细管柱,柱温:110℃;检测器:FID;进样口温度:200℃,检测器温度:250℃;载气:N2;流速:3.0 ml·min-1;分流进样;分流比:1∶1,以水为溶剂测定二氯乙烷,三氯甲烷残留量。结果:两种残留溶剂能够完全分离,二氯乙烷,三氯甲烷分别在0.25~2.52( r =0.9995),2.28~22.84μg·ml-1(r=0.9995)范围内,线性关系良好,平均回收率分别为98.4%,99.5%,RSD分别为1.14%和1.78%(n=9)。最低检出限分别为0.02,0.06μg·ml-1。结论:该顶空气相色谱法准确可靠,灵敏度高,可用于奥沙拉秦钠中残留溶剂的测定。
目的:改進奧沙拉秦鈉殘留溶劑的測定方法。方法:採用氣相色譜頂空進樣,色譜柱為DB-624彈性毛細管柱,柱溫:110℃;檢測器:FID;進樣口溫度:200℃,檢測器溫度:250℃;載氣:N2;流速:3.0 ml·min-1;分流進樣;分流比:1∶1,以水為溶劑測定二氯乙烷,三氯甲烷殘留量。結果:兩種殘留溶劑能夠完全分離,二氯乙烷,三氯甲烷分彆在0.25~2.52( r =0.9995),2.28~22.84μg·ml-1(r=0.9995)範圍內,線性關繫良好,平均迴收率分彆為98.4%,99.5%,RSD分彆為1.14%和1.78%(n=9)。最低檢齣限分彆為0.02,0.06μg·ml-1。結論:該頂空氣相色譜法準確可靠,靈敏度高,可用于奧沙拉秦鈉中殘留溶劑的測定。
목적:개진오사랍진납잔류용제적측정방법。방법:채용기상색보정공진양,색보주위DB-624탄성모세관주,주온:110℃;검측기:FID;진양구온도:200℃,검측기온도:250℃;재기:N2;류속:3.0 ml·min-1;분류진양;분류비:1∶1,이수위용제측정이록을완,삼록갑완잔류량。결과:량충잔류용제능구완전분리,이록을완,삼록갑완분별재0.25~2.52( r =0.9995),2.28~22.84μg·ml-1(r=0.9995)범위내,선성관계량호,평균회수솔분별위98.4%,99.5%,RSD분별위1.14%화1.78%(n=9)。최저검출한분별위0.02,0.06μg·ml-1。결론:해정공기상색보법준학가고,령민도고,가용우오사랍진납중잔류용제적측정。
Objective:To improve the determination method for the residual solvents in olsalazine sodium. Methods:1,2-Dichlo-roethane and chloroform were determined by headspace GC with a DB-624 capillary column and an FID detector. The column tempera-ture was 110℃. The temperature of the injector and the detector was 200℃ and 250℃, respectively. The carrier gas was nitrogen with a flow of 3. 0 ml·min-1 . The split ratio was 1∶1. Water was used as the solvent. Results:1,2-Dichloroethane and chloroform were completely separated with good linearity within the respective range of 0. 25-2. 52 ( r =0. 999 5 ) and 2. 28-22. 84 μg · ml-1 ( r =0. 999 5). The average recoveries were 98. 4% and 99. 5% with RSD of 1. 14% and 0. 98%(n=9), respectively. The detection lim-it were 0. 02 and 0. 06 μg·ml-1 , respectively. Conclusion:The method is rapid, sensitive and accurate, which can be used in the determination of residual organic solvents in olsalazine sodium.