Determination of Residual Solvents in α-Ketophenylalanine Calcium by Gas Chromatography
- VernacularTitle:气相色谱法测定α-酮苯丙氨酸钙中有机溶剂残留量
- Author:
Xiaoyi SHI
;
Yi LIU
;
Ke ZHANG
- Publication Type:Journal Article
- Keywords:
GC;
α-Ketophenylalanine calcium;
Residual solvents
- From:
China Pharmacist
2015;(8):1411-1412,1413
- CountryChina
- Language:Chinese
-
Abstract:
To develop a method for the determination of residual solvents inα-ketophenylalanine calcium by capillary gas chromatography. Methods:The residual solvents were separated on a DB-624(30 m × 0. 32 mm, 0. 25 μm) capillary chromato-graphic column with temperature programming. The column temperature was maintained at 40℃ for 1 min,and then raised to 180℃at a rate of 10℃·min-1 and maintained for 2 min. N2 was used as the carrier gas, and FID was used as the detector with temperature of 250 ℃. The injector temperature was 200 ℃ and the split ratio was 10∶1, and direct injection was adopted. Methanol, ethanol, ethyl acetate and tetrahydrofuran in α-ketoleucine calcium were detected using an external standard method. Results:The four solvents were separated completely. There was a good linear relationship between the peak area and the concentration of each solvent ( r=0. 997 2-0. 999 5). The average recovery of the four solvents was 95. 47%-100. 26%(RSD≤4. 7%, n=9). Conclusion:The method is rap-id, simple, accurate and sensitive, and can be used in the determination of residual solvents in α-ketophenylalanine calcium.