Beach Daniel G, Walsh Callee M, McCarron Pearse
National Research Council Canada, Measurement Science and Standards, 1411 Oxford Street, Halifax, NS, B3H 3Z1, Canada.
Protea Biosciences Group, Inc., 955 Hartman Run Road, Morgantown, WV, 26505, USA.
Toxicon. 2014 Dec 15;92:75-80. doi: 10.1016/j.toxicon.2014.10.009. Epub 2014 Oct 15.
Eliminating sample extraction or liquid chromatography steps from methods for analysis of the neurotoxin Domoic Acid (DA) in shellfish could greatly increase throughput in food safety testing laboratories worldwide. To this end, we have investigated the use of Laser Ablation Electrospray Ionization (LAESI) with tandem mass spectrometry (MS/MS) detection for DA analysis directly from mussel tissue homogenates without sample extraction, cleanup or separation. DA could be selectively detected directly from mussel tissue homogenates using MS/MS in selected reaction monitoring scan mode. The quantitative capabilities of LAESI-MS/MS for DA analysis from mussel tissue were evaluated by analysis of four mussel tissue reference materials using matrix-matched calibration. Linear response was observed from 1 mg/kg to 40 mg/kg and the method limit of detection was 1 mg/kg. Results for DA analysis in tissue within the linear range were in good agreement with two established methods, LC-UV and LC-MS/MS (recoveries from 103 to 125%). Beyond the linear range, extraction and clean-up were required to achieve good quantitation. Most notable is the extremely rapid analysis time of about 10 s per sample by LAESI-MS/MS, which corresponds to a significant increase in sample throughput compared with existing methodology for routine DA analysis.
从贝类中神经毒素软骨藻酸(DA)的分析方法中去除样品提取或液相色谱步骤,可大幅提高全球食品安全检测实验室的通量。为此,我们研究了使用激光烧蚀电喷雾电离(LAESI)结合串联质谱(MS/MS)检测,直接从贻贝组织匀浆中分析DA,而无需进行样品提取、净化或分离。在选择反应监测扫描模式下,使用MS/MS可直接从贻贝组织匀浆中选择性检测到DA。通过使用基质匹配校准分析四种贻贝组织参考物质,评估了LAESI-MS/MS对贻贝组织中DA分析的定量能力。在1 mg/kg至40 mg/kg范围内观察到线性响应,方法检测限为1 mg/kg。线性范围内组织中DA分析的结果与两种既定方法LC-UV和LC-MS/MS高度一致(回收率为103%至125%)。超出线性范围时,需要进行提取和净化以实现良好的定量。最值得注意的是,LAESI-MS/MS每个样品的分析时间极快,约为10秒,与常规DA分析的现有方法相比,这意味着样品通量显著提高。