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高效液相色谱法测定血浆中莲心碱

[Determination of liensinine in plasma by high performance liquid chromatography].

作者信息

Zhang X, Wen W, Hu X, Luo S, Cai H

机构信息

Department of Pharmacy, Hubei Medical University, Wuhan, 430060.

出版信息

Se Pu. 1997 Jul;15(4):347-8.

PMID:15739474
Abstract

A sensitive method of high performance liquid chromatography (HPLC) for determination of liensinine in plasma is reported. An Ultrasphere Si column, 250 mm x 4.6 mm i.d. with dichloromethaneisopropyl alcohol-diethylamine (75:25:0.2, V/V) as mobile phase at a flow-rate of 1.0 mL/min and UV-detector at 282 nm were used. Neferine was served as the internal standard. Liensinine in plasma was extracted with diethyl ether three times after adding ammonia-ammonium chloride buffer (pH 10). Liensinine was completely separated from nefrine. The retention times of liensinine and neferine were 8.5 and 5.0 minutes, respectively. The calibration line of liensinine was linear in the range of 0.0625-5.0 mg/L (r = 0.9996). The mean recovery was 93.6% with RSD of 1.9%. The precision of intra-day and inter-day for liensinine was in the range of 1.4%-4.1% and the detectable limit was 0.025 mg/L based on a signal-to-noise ratio of 3. The results showed that the method was simple and sensitive.

摘要

报道了一种测定血浆中莲心碱的高效液相色谱(HPLC)灵敏方法。采用内径为4.6 mm、长250 mm的Ultrasphere Si柱,以二氯甲烷 - 异丙醇 - 二乙胺(75:25:0.2,V/V)为流动相,流速为1.0 mL/min,在282 nm波长处用紫外检测器。以甲基莲心碱作为内标。在加入氨 - 氯化铵缓冲液(pH 10)后,用乙醚对血浆中的莲心碱萃取3次。莲心碱与甲基莲心碱完全分离。莲心碱和甲基莲心碱的保留时间分别为8.5分钟和5.0分钟。莲心碱的校准曲线在0.0625 - 5.0 mg/L范围内呈线性(r = 0.9996)。平均回收率为93.6%,相对标准偏差为1.9%。莲心碱日内和日间精密度在1.4% - 4.1%范围内,基于信噪比为3时的检测限为0.025 mg/L。结果表明该方法简便灵敏。

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1
[Determination of liensinine in plasma by high performance liquid chromatography].高效液相色谱法测定血浆中莲心碱
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Separation, identification and rapid determination of liensine, isoliensinine and neferine from embryo of the seed of Nelumbo nucifera Gaertn. by liquid chromatography coupled to diode array detector and tandem mass spectrometry.利用液相色谱-二极管阵列检测器-串联质谱联用技术对莲子胚中的莲心碱、异莲心碱和荷叶碱进行分离、鉴定和快速测定。
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