超高效液相色谱法测定辛伐他汀胶囊中叔丁基-4-羟基茴香醚与2,6-二叔丁基对甲酚的含量

摘要

Objective To establish a method for analysis of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in Simvastatin Capsules. Methods The chromatographic conditions included ACQUITY UPLCTM BEH C18 column (50 mm X 2. 1 mm, 1. 7 μm) ,mobile phase of acetonitrile(B) ;0. 005 mol o L-1 ammonium acetate(A) with gradient elution:0 min,60 : 40 ;2 min, 60 = 40; 5 min, 90 = 10; 8 min, 90 = 10; 9 min, 60 = 40; 10 min, 60 = 40 at a flow rate of 0. 25 mL o min-1 , the detection wavelength 280 nm,and the column temperature 40 °C. Results Good resolution for BHA,BHT and vitamin C was obtained. The limit of detection for BHA was 0. 5 ng,the linear range was 0. 203 5-50. 88 μg o mL-1 (r=0. 999 9) ,and the average recovery was 98. 3% (RSD=1. 0%). The limit of detection for BHT was 0. 5 ng.the linear range was 0. 211 4-52. 84 μg o mL-1 (r=0. 999 9) ,and the average recovery was 97. 2%(RSD=0. 5%). Conclusion The method is rapid,specific,sensitive and economic.%目的 建立超高效液相色谱法同时测定辛伐他汀胶囊中的抗氧剂叔丁基-4-羟基茴香醚(BHA)与2,6-二叔丁基对甲酚(BHT).方法 色谱柱为ACQUITY UPLCTM BEH C18 (50 mm×2.1 mm,1.7 μm).以乙腈(A)-0.005 mol·L-1醋酸铵(B)为流动相,梯度洗脱程序为:0 min,60∶40;2 min,60∶40;5 min,90∶10;8 min,90∶10;9 min,60∶40;10 min,60∶40.检测波长为280 nm,流速为0.25 mL·min-1,柱温为40 ℃.结果 在该色谱条件下,BHA和BHT与维生素C峰均能良好分离.BHA的检出限为0.5 ng;质量浓度在0.203 5～50.88 μg·mL-1范围内与峰面积呈良好的线性关系,相关系数r=0.999 9;回收率为98.3%,RSD为1.0%.BHT的检出限为0.5 ng;质量浓度在0.211 4～52.84 μg·mL-1范围内与峰面积呈良好的线性关系,相关系数r=0.999 9;回收率为97.2%,RSD为0.5%.结论 该方法快速、专属、灵敏度高,并且节能环保.