Xu Chun-lei, Chen Jian-wei, Ju Wen-zheng, Liu Shi-jia, Chen Yong, Chen Zhi-peng, Xue Ping, Chen Hong-jiang, Li Xiang
College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, People's Republic of China.
Biomed Chromatogr. 2012 Oct;26(10):1210-4. doi: 10.1002/bmc.2681. Epub 2011 Dec 30.
A rapid, sensitive and specific method using liquid chromatography with tandem mass spectrometric detection (LC-MS) was developed for the analysis of sauchinone in rat plasma. Di-O-methyltetrahydrofuriguaiacin B was used as internal standard (IS). Analytes were extracted from rat plasma by liquid-liquid extraction using ethyl acetate. A 2.1 mm i.d. × 150 mm, 5 µm, Agilent Zorbax SB-C(18) column was used to perform the chromatographic analysis. The mobile phase was methanol-deionized water (80:20, v/v). The chromatographic run time was 7 min per injection and the flow-rate was 0.2 mL/min. The tandem mass spectrometric detection mode was achieved with electrospray ionization interface in positive-ion mode (ESI(+) ). The m/z ratios M + Na , m/z 379.4 for sauchinone and m/z 395.4 for IS were recorded simultaneously. Calibration curve were linear over the range of 0.01-5 µg/mL. The lowest limit of quantification was 0.01 µg/mL. The intra-day and inter-day precision and accuracy of the quality control samples were 2.94-9.42% and 95.79-108.05%, respectively. The matrix effect was 64.20-67.34% and the extraction recovery was 93.28-95.98%. This method was simple and sensitive enough to be used in pharmacokinetic research for determination of sauchinone in rat plasma.
建立了一种采用液相色谱-串联质谱检测（LC-MS）的快速、灵敏且特异的方法，用于分析大鼠血浆中的柳杉酚。二-O-甲基四氢呋喃愈创木酚B用作内标（IS）。通过用乙酸乙酯进行液-液萃取从大鼠血浆中提取分析物。使用内径2.1 mm×150 mm、5 µm的安捷伦Zorbax SB-C(18)柱进行色谱分析。流动相为甲醇-去离子水（80:20，v/v）。每次进样的色谱运行时间为7分钟，流速为0.2 mL/分钟。采用电喷雾电离接口在正离子模式（ESI(+)）下实现串联质谱检测模式。同时记录柳杉酚的m/z比M + Na、m/z 379.4和内标的m/z 395.4。校准曲线在0.01 - 5 µg/mL范围内呈线性。最低定量限为0.01 µg/mL。质量控制样品的日内和日间精密度及准确度分别为2.94 - 9.42%和95.79 - 108.05%。基质效应为64.20 - 67.34%，提取回收率为93.28 - 95.98%。该方法简单且灵敏，足以用于大鼠血浆中柳杉酚测定的药代动力学研究。
