Determination of 9 Residual Organic Solvents in Blonanserin by Headspace Gas Chromatography
10.6039/j.issn.1001-0408.2017.12.32
- VernacularTitle:顶空气相色谱法同时测定布南色林原料药中9种有机溶剂的残留量
- Author:
Lijuan PEI
;
Chen TIAN
;
Ranran QI
;
Zhuo ZHANG
;
Ye WANG
- Keywords:
Blonanserin;
Headspace gas chromatography;
Residual organic;
Methanol;
Alcohol;
Isopropyl alcohol;
Acetoni-trile;
Dichloromethane;
Hexane;
Ethyl acetate;
Tetrahydrofuran;
Methylbenzene
- From:
China Pharmacy
2017;28(12):1699-1702
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for the determination of 9 residual organic solvents in blonanserin as methanol, alcohol,isopropyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene. METHODS:Headspace gas chromatography was adopted. The determination was performed on DB-624 capillary column using temperature pro-gramming. The inlet temperature was 150 ℃,and flame ionization detector was used with temperature of 250 ℃. High purity nitro-gen was used as carrier gas with flow rate of 2.8 mL/min. The split ratio was 1:1,and headspace sample size was 1 mL. Head-space heating temperature was 90 ℃,and equilibration time was 35 min. RESULTS:The linear ranges of methanol,alcohol,iso-propyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene were 6-1500 μg/mL(r=0.9998),10-2500 μg/mL(r=0.9999),10-2500 μg/mL(r=0.9998),0.82-205 μg/mL(r=0.9994),1.2-300 μg/mL(r=0.9995), 0.58-145 μg/mL(r=0.9994),10-2500 μg/mL(r=0.9999),1.44-360 μg/mL(r=0.9996),1.78-445 μg/mL(r=0.9995),respec-tively. The limits of quantitation were 17.71,6.02,3.17,7.45,1.53,0.69,0.93,1.01,0.22 μg/mL;the limits of detection were 5.89,1.90,1.05,2.48,0.51,0.23,0.31,0.33,0.07 μg/mL,respectively. RSDs of precision and stability tests were all lower than 3.0%,and isopropanol was found in repeatability test (RSD=2.1%). The average recoveries ranged 96.67%-102.66%(RSD=1.9%,n=9),96.00%-101.83%(RSD=1.9%,n=9),97.17%-101.50%(RSD=1.4%,n=9),96.97%-102.44%(RSD=2.2%,n=9),95.83%-103.33%(RSD=2.5%,n=9),95.83%-100.28%(RSD=1.9%,n=9),98.17%-101.25%(RSD=1.0%,n=9),96.55%-102.30%(RSD=1.9%,n=9),96.30%-102.22%(RSD=1.8%,n=9),respectively. CONCLUSIONS:The method is simple,rapid,accurate and suitable for simultaneous determination of 9 residual organic solvents in blonanserin as methanol,alco-hol,isopropyl alcohol,acetonitrile,dichloromethane,hexane,ethyl acetate,tetrahydrofuran and methylbenzene.
