Nozaki Kazuyoshi, Osaka Issey, Kawasaki Hideya, Arakawa Ryuichi
Department of Applied Chemistry, Faculty of Chemistry, Materials and Bioengineering, Kansai University, 3-3-35 Yamate, Suita, Osaka 564-8680, Japan.
Anal Sci. 2009 Oct;25(10):1197-201. doi: 10.2116/analsci.25.1197.
A simple, rapid, and sensitive on-line liquid chromatographic electrochemistry/electrospray/tandem mass spectrometry (LC-EC/ESI-MS/MS) method for the determination of zotepine in human serum was developed using a new generated-electrochemically fragment ion, and was validated. A recent novel technique of LC-EC/ESI-MS/MS that combines LC-MS/MS and the on-line EC reaction is potentially applicable to developing a quantification method for drugs in biological samples. Newly formed products generated by the on-line EC cell are expected to provide appropriate precursor and product ions for the MS/MS determination method. This technique was successfully applied to a drug assay in a biological matrix. After adding imipramine (IS) to a 30-microL aliquot of human serum, the resulting sample was simply deproteinated with acetonitrile for a measurement. The analytical run time was 5 min. The calibration curve was linear in the concentration range of 10-2000 ng/mL. The intra-assay precision and accuracy were in the range of 1.8-8.9 and 98.4-113%, respectively.
建立了一种简单、快速、灵敏的在线液相色谱-电化学/电喷雾/串联质谱(LC-EC/ESI-MS/MS)法测定人血清中的佐替平,该方法采用新生成的电化学碎片离子,并进行了验证。最近一种结合LC-MS/MS和在线EC反应的新型LC-EC/ESI-MS/MS技术有可能应用于生物样品中药物定量方法的开发。在线EC池产生的新形成产物有望为MS/MS测定方法提供合适的前体和产物离子。该技术成功应用于生物基质中的药物分析。向30微升人血清等分试样中加入丙咪嗪(内标)后,所得样品用乙腈简单脱蛋白后进行测定。分析运行时间为5分钟。校准曲线在10-2000 ng/mL浓度范围内呈线性。批内精密度和准确度分别在1.8-8.9%和98.4-113%范围内。