Simultaneous Residual Determination of Two Organic Solvents in Bisacodyl Raw Material by Head-space GC
10.6039/j.issn.1001-0408.2016.30.39
- VernacularTitle:顶空气相色谱法同时测定比沙可啶原料药中2种溶剂残留量
- Author:
Jianguo JIANG
;
Ting SUN
;
Yonghui GUO
;
Xuejing HAN
;
Huijuan MIAO
- Publication Type:Journal Article
- Keywords:
Bisacodyl;
Head-space GC;
Residual determination;
Dichloromethane;
Ethyl acetate
- From:
China Pharmacy
2016;27(30):4297-4298,4299
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material. METHODS:Head-space GC was performed on the capillary column of 6% cyanopropyl phenyl-94% di-methyl polysiloxane(DB-624)by temperature programming,the temperature of injector was 220 ℃,detector was flame ionization detector with temperature of 250 ℃,carrier gas was high purity nitrogen with the flow rate of 3.0 ml/min,split ration was 1∶10, headspace heating temperature was 70 ℃,equilibration time was 30 min,volume of headspace vial was 5 ml,and the injection volume was 1 ml. RESULTS:The linear range was 6-120μg/ml for dichloromethane(r=0.999 9)and 50-1 000μg/ml for ethyl ac-etate(r=0.999 9);the limit of quantitation was 0.2,1.7 μg,limit of detection was 0.06,0.5 μg;RSDs of precision,stability and reproducibility tests were no higher than 3%;recoveries were 100.30%-102.00%(RSD=0.63%,n=9) and 100.10 %-101.30%(RSD=0.44%,n=9). CONCLUSIONS:The method is simple and accurate,and can be used for the simultaneous residual deter-mination of dichloromethane and ethyl acetate in bisacodyl raw material.
