UPLC-QQQ/MS法检测驴胶补血颗粒中的阿胶
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篇名: UPLC-QQQ/MS法检测驴胶补血颗粒中的阿胶
TITLE:
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 C18,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5 μL。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20.24~2 024 μg/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。
ABSTRACT: OBJECTIVE: To establish a method for the determination of donkey-hide gelatin in Lüjiao buxue granules. METHODS: Trypsin was used for enzymatic hydrolysis of donkey-hide gelatin. UPLC-QQQ/MS was adopted for the determination of donkey-hide gelatin in the preparation: Hypersil GOLD C18 column was used with mobile phase consisted of 0.1% formic acid solution-acetonitrile (gradient elution) at the flow rate of 0.3 mL/min. The column temperature was 30 ℃, and sample size was 5 μL. Mass chromatography condition was that ion source was electrospray ion source; ionization mode was ESI+; multiple response monitoring 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-hide gelatin ranged 20.24-2 024 μg/mL(r=0.997 8). The detection limit was 1%. RSDs of precision, stability and reproducibility tests were all lower than 6.0%. The characteristic molecular ion peaks of donkey-hide gelatin could be detected in 27 batches of samples. CONCLUSIONS: The method is specific and can be used for the determination of donkey-hide gelatin in Lüjiao buxue granules.
期刊: 2017年第28卷第15期
作者: 陈鸿玉,李劲平,李文莉,丁野,孙辉,杨清,黄晓燕
AUTHORS: CHEN Hongyu,LI Jinping,LI Wenli,DING Ye,SUN Hui,YANG Qing,HUANG Xiaoyan
关键字: 超高效液相色谱-三重四极杆质谱法;驴胶补血颗粒;阿胶;特征分子离子峰
KEYWORDS: UPLC-QQQ/MS; Lüjiao buxue granules; Donkey-hide gelatin; Characteristic molecular ion peak
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