HPLC法检测布舍瑞林注射液中防腐剂降解产物苯甲醛的含量

Degradation Product of preservatives in Buserelin Injection by HPLC

关键词:  布舍瑞林注射液  降解产物  高效液相色谱法  苯甲醇  苯甲醛

Key words:  Buserelin Injection  Degradation product  HPLC  Benzyl Alcohol  Benzaldehyde

摘要:

建立布舍瑞林注射液中防腐剂苯甲醇的降解产物苯甲醛的高效液相色谱检测方法。采用ODS–2 Hypersil色谱柱（4.6 mm×250 mm， 5 μm），以磷酸盐溶液（11.2 g·L-1磷酸溶液，用三乙胺调节pH值至2.5）–乙腈（77︰23）为流动相，流速1.0 mL·min-1，检测波长220 nm，柱温40 ℃，进样量100 μL。在此色谱条件下，测定的各批样品，苯甲醛含量均小于10 μg·mL-1，苯甲醛在1.010~14.140 μg·mL-1（r=0.999 6）范围内浓度与峰面积有良好的线性关系，检测限为3 ng·mL-1，定量限为10 ng·mL-1，平均回收率为101.82%。本方法准确度高，重复性好，可用于布舍瑞林注射液中苯甲醛的含量测定。

Abstract:

To establish a high-performance liquid chromatography (HPLC)method for the determination of benzaldehyde, a degradation product of benzyl alcohol,in buserelin injection as a preservative.The column was ODS-2 Hypersil column (4.6 mm×250 mm,5 μm).The mobile phase was phosphate buffer(11.2 g·L-1 phosphate acid solution, pH value was adjusted to 2.5 with triethylamine)-acetonitrile(77︰23).The flow rate was 1.0 mL·min-1.The detection wavelength was 220 nm.The column temperature was 40 ℃ and injection volume was 100 μL.Under the chromatographic conditions, the content of benzaldehyde in each batch of samples was less than 10 μg·mL-1, the concentration of benzaldehyde had a good linear relationship with peak area in the range of 1.010~14.140 μg·mL-1 (r=0.999 6) , the detection limit is 3 ng·mL-1 and the quantification limit is 10 ng·mL-1, and the average recovery rate was 101.82%.The method was accurate, reproducible, and can be used for the determination of benzaldehyde in Busherelin injection.