ABSTRACT
Objective:To establish an HPLC method for the determination of related substances in piperazine ferulate. Methods:An HPLC method was used to determine the related substances in piperazine ferulate. The separation was performed on an Xtimate C18 column (250 mm × 4. 6 mm, 5 μm). The mobile phase was 0. 5% acetic acid-methanol-acetonitrile with gradient elution. The flow rate was 1. 0 ml·min-1 and the column temperature was 30℃. The detection wavelength was 286 nm and the injection volume was 20μl. Results:Ferulic acid had a good linear relationship within the range of 5-30 μg·ml-1(r=1.0000). The detection limit was 0. 02 ng. Conclusion:The method is reliable, simple, accurate, stable and durable, and suitable for the determination of related sub-stances in piperazine ferulate.
ABSTRACT
Objective:To establish a method for the determination of benzene, chlorine alcohol and pyridine residues in piperazine ferulate. Methods:GC was used with a DB-624 (30 m × 0. 53 mm, 1. 0 μm) elastic quartz capillary column. The flame ionization detector was used with nitrogen as the carrier gas. The initial temperature was 50℃, maintaining for 5 min, and raised to 80℃ at the rate of 10℃·min-1 , and then raised to 200℃ at the rate of 50℃·min-1 , and maintaining for 4 minutes. The inlet temperature was 200℃, and the detector temperature was 220℃. The split ratio was 1 ∶1 and the injection volume was 1μl. The flow rate was 3 ml· min-1. Results:The linear range of benzene was 0.16-0.96 μg·ml-1(r=0.999 5), the average recovery was 95.7% (RSD =2.1, n=9), and the detection limit was 0.16 ng. The linear range of chlorine alcohol was 16.11-96.65 μg·ml-1(r=0.999 7), the average recovery was 97. 8% (RSD=2. 1, n=9), and the detection limit was 0. 62 ng. The linear range of pyridine was 15. 87-95. 23 μg·ml-1(r=0. 999 8), the average recovery was 99. 2% (RSD=1. 3, n=9), and the detection limit was 0. 15 ng. Con-clusion:The method is reliable, simple, accurate and stable, and suitable for the determination of benzene, chlorine alcohol and pyri-dine residues in piperazine ferulate.