Liang Mingjin, Zhang Weidong, Hu Jiang, Liu Runhui, Zhang Chuan
School of Pharmacy, Second Military Medical University, Shanghai 200433, PR China.
J Pharm Biomed Anal. 2006 Sep 18;42(2):178-83. doi: 10.1016/j.jpba.2006.03.031. Epub 2006 May 24.
The chemical profiles of nine alkaloids in Zanthoxylum nitidum, including berberubine, coptisine, sanguinarine, nitidine, chelerythrine, liriodenine, 6,7,8-trimethoxy-2,3-methylendioxybenzophenantridine, oxyavicine and dihydrochelerythrine, were identified by using high performance liquid chromatography-diode array detector-electrospray tandem mass spectrometry (HPLC-DAD-ESI-MS), and a novel and sensitive HPLC-UV method had been developed to simultaneously determine these alkaloids in 70% methanol extract of Zanthoxylum nitidum. The chromatographic separation was performed on an Agilent C(18) analytical column (5 microm, 4.6 mm i.d., 250 mm length) with a gradient solvent system of acetonitrile-0.1% formic buffer (adjusted to pH 4.5 with triethylamine). The methodological validation was carried out and the linearities (r(2)>0.9997) and recoveries (ranged from 98.3% to 101.1%) were acceptable. The limits of detection (LOD) of these alkaloids were ranged from 0.6 ng to 1.5 ng. The results indicated that the contents of alkaloids in Zanthoxylum nitidum varied significantly from habitat to habitat with contents ranged from 0.03 mg/g to 3.34 mg/g. The proposed method is simple, effective and suitable for the quality control of this traditional Chinese medicine (TCM). It suggests that it is necessary to control its quality so as to insure efficacy and safety of TCM.
采用高效液相色谱 - 二极管阵列检测器 - 电喷雾串联质谱法（HPLC - DAD - ESI - MS）鉴定了两面针中9种生物碱的化学特征，包括小檗红碱、黄连碱、血根碱、氧化两面针碱、白屈菜红碱、鹅掌楸碱、6,7,8 - 三甲氧基 - 2,3 - 亚甲二氧基苯菲啶、氧化阿魏碱和二氢白屈菜红碱，并建立了一种新颖、灵敏的HPLC - UV方法，用于同时测定两面针70%甲醇提取物中的这些生物碱。色谱分离在Agilent C(18)分析柱（5μm，内径4.6mm，长250mm）上进行，采用乙腈 - 0.1%甲酸缓冲液（用三乙胺调至pH 4.5）的梯度溶剂系统。进行了方法学验证，线性关系（r(2)>0.9997）和回收率（98.3%至101.1%）均可接受。这些生物碱的检测限（LOD）在0.6 ng至1.5 ng之间。结果表明，两面针中生物碱的含量因产地不同而有显著差异，含量范围为0.03 mg/g至3.34 mg/g。所建立的方法简便、有效，适用于该中药的质量控制。这表明有必要控制其质量以确保中药的疗效和安全性。
