OBJECTIVE: To establish a method for simultaneous determination of 6 residual organic solvents in aprepitant raw material as methanol, ethanol, acetone, isopropyl alcohol, methyl tert-butyl ether and tetrahydrofuran. METHODS: Headspace capillary gas chromatography was adopted. The determination was performed on DB-624 capillary column using temperature progra- mming. The temperature of injector port was 180 ℃, and flame ionization detector was used with temperature of 260 ℃. Nitrogen was used as carrier gas with flow rate 3.0 mL/min. The spilt ratio was 5 ∶ 1, and head-space injection volume was 1.0 mL. The head-space equilibrium temperature was set at 80 ℃, and equilibrium time was 40 min. RESULTS:The linear ranges of methanol, ethanol, acetone, isopropyl alcohol, methyl tert-butyl ether, tetrahydrofuran were 6.052-605.232 μg/mL(r=0.999 9), 9.987-998.718 μg/mL(r=0.999 9), 9.998-999.768 μg/mL(r=0.999 8), 9.986-998.634 μg/mL(r=0.999 9), 9.991-999.090 μg/mL(r=0.999 7), 1.461-146.133 μg/mL(r=0.999 5), respectively. The limits of quantitation were 1.782 1,2.079 0,0.749 8,1.777 8, 0.223 1,0.607 0 μg/mL; the limits of detection were 0.594 0,0.693 0,0.249 9,0.592 6,0.074 4, 0.202 3 μg/mL, respectively. RSD of precision test was lower than 2.0%. Only acetone and isopropyl alcohol were detected in stability test and reproducibility tests,RSD<2.0%. Their recoveries were 99.34-100.75%(RSD=0.52%,n=9),98.20%-100.24%(RSD=0.69%,n=9), 98.07%-100.07%(RSD=0.84%,n=9), 99.86%-101.32%(RSD=0.58%,n=9),97.87%-104.02%(RSD=2.13%,n=9), 98.26%-100.58%(RSD=0.75%,n=9), respectively. CONCLUSIONS: The established method is simple, accurate and reproducible, and can be used for simultaneous determination of 6 residual organic solvents in aprepitant raw material.
关键词
顶空毛细管气相色谱法阿瑞匹坦有机溶剂残留量
Keywords
Headspace capillary gas chromatographyAprepitantOrganic solventResidual