中国药师
中國藥師
중국약사
CHINA PHARMACIST
2015年
5期
865-866,867
,共3页
丹酚酸B%有机溶剂残留%顶空气相色谱法
丹酚痠B%有機溶劑殘留%頂空氣相色譜法
단분산B%유궤용제잔류%정공기상색보법
Salvianolic acid B%Residual organic solvent%Headspace GC
目的：：建立丹酚酸B原料药中3种残留溶剂的测定方法。方法：采用顶空毛细管气相色谱法测定,色谱柱为HP-5毛细管柱(30 m ×0.32 mm,0.6μm),进样口温度为180℃,进样量为0.1 ml,分流比为1∶10；柱温为40℃保持6 min,15℃· min-1升温至180℃,保持5 min；检测器为FID,温度：250℃；载气：N2,流速：1.7 ml·min-1。二甲亚砜(DMSO)为溶剂。结果：各残留溶剂均可达到基线分离。各残留溶剂乙醇、丙酮和乙酸乙酯分别在12.650~1.012×103μg·ml-1(r =0.9993)、12.750~1.020×103μg·ml-1(r=0.9997)、12.550~1.004×103μg·ml-1(r=0.9997)范围内线性关系良好。乙醇、丙酮、乙酸乙酯的平均回收率分别为96.89%(RSD=3.81%,n=9)、99.56%(RSD=4.05%,n=9)、97.21%(RSD=4.95%,n=9)。结论：该法操作简便,重复性好,结果准确可靠,可以用于丹酚酸B原料药中残留溶剂的测定。
目的：：建立丹酚痠B原料藥中3種殘留溶劑的測定方法。方法：採用頂空毛細管氣相色譜法測定,色譜柱為HP-5毛細管柱(30 m ×0.32 mm,0.6μm),進樣口溫度為180℃,進樣量為0.1 ml,分流比為1∶10；柱溫為40℃保持6 min,15℃· min-1升溫至180℃,保持5 min；檢測器為FID,溫度：250℃；載氣：N2,流速：1.7 ml·min-1。二甲亞砜(DMSO)為溶劑。結果：各殘留溶劑均可達到基線分離。各殘留溶劑乙醇、丙酮和乙痠乙酯分彆在12.650~1.012×103μg·ml-1(r =0.9993)、12.750~1.020×103μg·ml-1(r=0.9997)、12.550~1.004×103μg·ml-1(r=0.9997)範圍內線性關繫良好。乙醇、丙酮、乙痠乙酯的平均迴收率分彆為96.89%(RSD=3.81%,n=9)、99.56%(RSD=4.05%,n=9)、97.21%(RSD=4.95%,n=9)。結論：該法操作簡便,重複性好,結果準確可靠,可以用于丹酚痠B原料藥中殘留溶劑的測定。
목적：：건립단분산B원료약중3충잔류용제적측정방법。방법：채용정공모세관기상색보법측정,색보주위HP-5모세관주(30 m ×0.32 mm,0.6μm),진양구온도위180℃,진양량위0.1 ml,분류비위1∶10；주온위40℃보지6 min,15℃· min-1승온지180℃,보지5 min；검측기위FID,온도：250℃；재기：N2,류속：1.7 ml·min-1。이갑아풍(DMSO)위용제。결과：각잔류용제균가체도기선분리。각잔류용제을순、병동화을산을지분별재12.650~1.012×103μg·ml-1(r =0.9993)、12.750~1.020×103μg·ml-1(r=0.9997)、12.550~1.004×103μg·ml-1(r=0.9997)범위내선성관계량호。을순、병동、을산을지적평균회수솔분별위96.89%(RSD=3.81%,n=9)、99.56%(RSD=4.05%,n=9)、97.21%(RSD=4.95%,n=9)。결론：해법조작간편,중복성호,결과준학가고,가이용우단분산B원료약중잔류용제적측정。
Objective:To establish a method to determine the residual solvents in salvianolic acid B. Methods: The headspace GC was carried out on an HP-5 capillary column(30 m × 0. 32 mm,0. 6 μm). The inlet temperature was 180℃. The injection volume was 0. 1ml and the separation ratio was 1:10. The column temperature was programmed:the initial temperature was 40℃, malntalned for 6 min, ralsed to 180℃ with a rate of 15 ℃·min-1 , and malntalned for another 5 min. The detector was FID with the temperature of 250℃. The carrier gas was N2 with the flow rate of 1. 7 ml·min-1 . DMSO was used as the solvent for salvianolic acid B. Results:All solvents could be separated completely. The linear range of ethanol, acetone and ethyl acetate was 12. 650-1. 012 × 103 μg·ml-1 (r=0.999 3),12.750-1.012 ×103 μg·ml-1(r=0.999 7) and 12.550-1.004 ×103 μg·ml-1(r=0.999 7), respectively. The average recovery of ethanol, acetone and ethyl acetate was 96. 89% (RSD=3. 81%,n=9), 99. 56% (RSD=4. 05%,n=9) and 97. 21% (RSD=4. 95%,n=9), respectively. Conclusion:The method is simple, reproducible and accurate enough for the determi-nation of residual solvents in salvianolic acid B.
