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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 |
| 阅读数： | 415 次 |
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