论文部分内容阅读
舒肝祛脂胶囊是新华医院的院内中药复方制剂,临床主要用于脂肪肝引起的转氨酶升高和肝内脂肪浸润,肥胖、高血脂等疾病治疗。本文建立了一种UHPLC-MS/MS方法可同时测定舒肝祛脂胶囊中的三七皂苷R1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rg1等4种三七皂苷成分的含量。色谱柱采用ZORBAX SB-C18(2.1 mm×50 mm,1.8μm),流动相为(0.05%甲酸+5 mM醋酸铵)水溶液–乙腈,梯度洗脱,流速为0.3 mL/min,柱温40 ℃质谱采用电喷雾离子源(ESI),多反应离子监测(MRM),并结合正负离子扫描切换,其中人参皂苷Re、人参皂苷Rg1采用负离子模式检测,三七皂苷R1、人参皂苷Rb1及内标人参皂苷F1采用正离子模式检测。结果显示三七皂苷R1、人参皂苷Rb1、人参皂苷Re、人参皂苷Rg1的定量限分别为6.54×10–4 ng/mL、2.57×10–4 ng/mL、0.11 ng/mL、6.91×10–3 ng/mL,检测限分别为1.96×10–4 ng/mL、7.70×10–5 ng/mL、3.45×10–2 ng/mL、2.07×10–3 ng/mL。在相应的线性范围内r 2>0.9633日内和日间精密度(RSD)均小于5%,平均回收率均在80%–120%。本方法在6 min内实现这4种皂苷成分的分离和测定,简单、快速、灵敏、准确,可用于舒肝祛脂胶囊中皂苷类成分的含量测定。
Shugan Quzhi Capsule Xinhua Hospital hospital compound prescriptions, clinical mainly for fatty liver caused by elevated transaminases and intrahepatic fatty infiltration, obesity, hyperlipidemia and other diseases. This article established a UHPLC-MS / MS method for the simultaneous determination of three kinds of notoginsenoside R1, ginsenoside Rb1, ginsenoside Re, ginsenoside Rg1 and other four kinds of notoginsenoside content of Shugan Quzhi Capsules. The column was eluted with a gradient of ZORBAX SB-C18 (2.1 mm × 50 mm, 1.8 μm) and a mobile phase of acetonitrile (0.05% formic acid + 5 mM ammonium acetate) - acetonitrile at a flow rate of 0.3 mL / Mass spectrometry was performed with electrospray ionization (ESI), multi-reactive ion monitoring (MRM) and positive-negative ion scan switching. Ginsenoside Re and ginsenoside Rg1 were detected by negative ion mode. Notoginsenoside R1, ginsenoside Rb1 and internal standard ginseng Saponin F1 was detected using positive mode. The results showed that the quantitative limits of notoginsenoside R1, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 were 6.54 × 10-4 ng / mL, 2.57 × 10-4 ng / mL, 0.11 ng / mL and 6.91 × 10- The detection limits were 1.96 × 10-4 ng / mL, 7.70 × 10-5 ng / mL, 3.45 × 10-2 ng / mL and 2.07 × 10-3 ng / mL, respectively. Within the corresponding linear range, r 2> 0. 9633 Intra-day and inter-day precision (RSD) were less than 5%, and the average recovery was between 80% and 120%. The method can realize the separation and determination of the four saponin components within 6 min, which is simple, rapid, sensitive and accurate and can be used for determining the content of saponins in Shugan Quzhi Capsules.