目的:建立柱前衍生-HPLC 法测定氨咖黄敏胶囊中6 个效应成分(对乙酰氨基酚、咖啡因、马来酸氯苯那敏、胆红素、胆酸、猪去氧胆酸)及2 个杂质成分(对氨基酚和对氯苯乙酰胺)的含量。方法:以2-萘基溴甲基酮为衍生剂,三乙胺为催化剂,以0.02% 醋酸溶液(A)-甲醇(B)-乙腈(C)为流动相,以265 nm 和446 nm(胆红素)为检测波长,对各成分进行梯度洗脱。结果:对乙酰氨基酚在49.62~620.24 μg·mL-1 浓度范围内线性良好(r=0.999 0),咖啡因在3.29~41.10 μg·mL-1 浓度范围内线性良好(r=0.999 6),马来酸氯苯那敏在0.21~2.59 μg·mL-1 浓度范围内线性良好(r=0.999 4),胆红素在1.30~16.28 μg·mL-1 浓度范围内线性良好(r=0.999 6),胆酸衍生物在2.64~32.94 μg·mL-1 浓度范围内线性良好(r=0.998 5),猪去氧胆酸衍生物在2.77~34.58 μg·mL-1 浓度范围内线性良好(r=0.999 2),对氨基酚在0.26~3.19 μg·mL-1 浓度范围内线性良好(r=0.999 8),对氯苯乙酰胺在0.22~2.82 μg·mL-1 浓度范围内线性良好(r0.999 9); 回收率均值(n=9)分别为：100.3%(RSD=0.98%)、102.0%(RSD=1.0%)、101.1%(RSD=1.3%)、99.86% (RSD=0.70%)、99.6%(RSD=1.4%)、103.0%(RSD=2.2%)、100.7%(RSD=1.2%)、100.51%(RSD=1.4%)。结论:该方法适用于对氨咖黄敏胶囊的主成分的含量测定及杂质测定。
Objective: To establish a pre-column derivatization-HPLC method for the determination of 6 bioactive components(acetaminophen,caffeine,chlorphenamine maleate,bilirubin,cholic acid,hyodeoxycholic acid)and 2 impurities(p-aminophenol,p-chloroacetanilide)in ACAC capsules. Methods: 2-Naphthyl bromomethyl ketone was used as the derivative,triethylamine was used as the catalyst and 0.02% acetic acid solution(A-methanol(B)-acetonitrile(C)was prepared as the mobile phase. The detection wavelengths were 265 nm and 446 nm(bilirubin). Results: Acetaminophen showed a good linearity in the range of 49.62-620.24 μg·mL-1(r=0.999 0);caffeine showed a good linearity in the range of 3.29-41.10 μg·mL-1(r=0.999 6);chlorphenamine maleate showed a good linearity in the range of 0.21-2.59 μg·mL-1(r=0.999 4);bilirubin showed a good linearity in the range of 1.30-16.28 μg·mL-1(r=0.999 6);cholic acid derivative showed a good linearity in the range of 2.64-32.94 μg·mL-1 (r=0.998 5);hyodeoxycholic acid derivative showed a good linearity in the range of 2.77-34.58 μg·mL-1(r=0.999 2); p-aminophenol showed a good linearity in the range of 0.26~3.19 μg·mL-1(r=0.999 8); p-chloroacetanilide showed a good linearity in the range of 0.22-2.82 μg·mL-1(r=0.999 9). The average recoveries(n=9)were 100.3% (RSD=0.98%), 102.0%(RSD=1.0%), 101.1%(RSD=1.3%), 99.9%(RSD=0.70%), 99.6%(RSD=1.4%), 103, 0%, (RSD=2.2%), 100.7%,(RSD=1.2%)and100.5%(RSD=1.4%)respectively. Conclusion: This method is suitable for the content determination of the main components and impurities in ACAC capsules.
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