A modified LC-MS/MS method for determination of tetramethylpyrazine in microdialysis samples and calibration of home-made linear probes
A modified LC-MS/MS method for determination of tetramethylpyrazine in microdialysis samples and calibration of home-made linear probes
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一种改进的 LC-MS/MS 方法，用于测定微透析样品中的四甲基吡嗪并校准自制线性探针。
DOI：
10.1002/bmc.2689
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发表时间：
2012-10-01
影响因子：
1.8
通讯作者：
Chen, Fang
中科院分区：
文献类型：
--
作者：
Han, Jin-Zhao;Sun, Jun;Chen, Fang
川芎嗪（Tetramethylpyrazine， TMP）是中药川芎（Ligusticum wallichii Franchat）中最重要的活性成分之一，被广泛用于心血管疾病的治疗。几个因素可能影响局部给药后TMP暴露，导致很大的变异性，需要进一步阐明药物分布。本文描述了一种新的高效可靠的LC-MS/MS测定皮肤微析液中TMP的方法，其中TMP在Agilent C（18）柱（3.5µm, 100 mm × 2.1 mm i.d）上分离，使用甲醇，水和乙酸的混合物（50:50:0.6,v/v/v），流速为0.3 mL/min。TMP的保留时间为1.89 min，内标（咖啡因）的保留时间为1.17 min。组织学分析证实了对微透析探针的炎症反应和胶原蛋白胶囊的存在。TMP的膜提取效率（输送到组织空间的百分比）在种植寿命期间没有改变。验证和样品分析结果表明，该方法精密度高，准确度高，适合支持皮肤微透析实验。
Tetramethylpyrazine (TMP) is one of the most important active ingredients of a Chinese herb Ligusticum wallichii Franchat, which is widely used for the treatment of cardiovascular diseases. Several factors may affect TMP exposure after topical administration, resulting in large variability and demanding further elucidation of drug distribution. This paper describes a new efficient reliable LC-MS/MS assay for the determination of TMP in dermal microdialysate, where TMP was separated on an Agilent C(18) column (3.5 µm, 100 mm × 2.1 mm i.d.) using a mixture of methanol, water and acetic acid (50:50:0.6, v/v/v) at a flow-rate of 0.3 mL/min. The retention time was 1.89 min for TMP and 1.17 min for the internal standard (caffeine). Histological analysis confirmed an inflammatory response to the microdialysis probes and the presence of a collagen capsule. The membrane extraction efficiency (percentage delivered to the tissue space) for TMP was not altered through the implant lifetime. The validation and sample analysis results showed that the method is precise, accurate and well suited to support dermal microdialysis experiments.