摘要
目的:建立驴胶补血颗粒中阿胶的检测方法。方法:采用胰蛋白酶对制剂中阿胶进行酶解,并采用超高效液相色谱-三重四极杆质谱联用法检测制剂中阿胶成分。色谱条件:色谱柱为Hypersil GOLD C_(18),流动相为0.1%甲酸溶液-乙腈(梯度洗脱),流速为0.3 mL/min,柱温为30℃,进样量为5μL。质谱条件:离子源为电喷雾离子源,离子化模式为电喷雾正离子化模式(多反应监测),检测离子对为阿胶特征分子离子峰m/z 539.8(双电荷)→612.4和m/z 539.8(双电荷)→923.8,喷雾电压为3 100 V,鞘气压为20 Arb,辅助气压为8 Arb,离子传热管温度为350℃,蒸发温度为350℃,扫描模式为单离子检测扫描,碰撞气体为高纯氩气。结果:阿胶成分检测质量浓度线性范围为20.24~2 024μg/mL(r=0.997 8);检测限为1%;精密度、稳定性、重复性试验的RSD<6.0%。27批样品中均检出阿胶特征分子离子峰。结论:该方法专属性强,可用于驴胶补血颗粒中阿胶的检测。
OBJECTIVE： To establish a method for the determination of donkey-hide gelatin in Liijiao buxue granules. METH- ODS ： Trypsin was used for enzymatic hydrolysis of donkey-hide gelatin. UPLC-QQQ/MS was adopted for the determination of don- key-hide gelatin in the preparation： Hypersil GOLD C18 column was used with mobile phase consisted of 0.1% formic acid solu- tion-acetonitrile （gradient elution） at the flow rate of 0.3 mL/min. The column temperature was 30℃, and sample size was 5μL. Mass chromatography condition was that ion source was electrospray ion source; ionization mode was ESI＋; multiple response mon- itoring was adopted, and characteristic molecular ion peaks of donkey-hide gelatin with mass-to-charge ratio of m/z 539.8 （double charge） 612.4 and m/z 539.8 （double charge） → 923.8 were used as detection ion pair. Spray voltage was 3 100 V; sheath gas was 20 Arb; auxiliary gas was 8 Arb; ion transfer tube temperature was 350℃ ; evaporation temperature was 350℃ ; scan mode was SRM. Collision gas was high purity argon. RESULTS： The sample size of donkey-bide gelatin ranged 20.24-2 024μg/mL（r= 0.997 8）. The detection limit was 1%. RSDs of precision, stability and reproducibility tests were all lower than 6.0%. The charac- teristic molecular ion peaks of donkey-hide gelatin could be detected in 27 batches of samples. CONCLUSIONS： The method is spe- cific and can be used for the determination of donkey-hide gelatin in LOjiao buxue granules.
出处
《中国药房》
CAS
北大核心
2017年第15期2101-2104,共4页
China Pharmacy
基金
国家科技重大专项课题(No.2014ZX09304307)
湖南省食品药品监督管理局食品药品安全科技项目(No.湘食药科R201504)
