The determination of melamine in muscle tissue by liquid chromatography/tandem mass spectrometry
The determination of melamine in muscle tissue by liquid chromatography/tandem mass spectrometry
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DOI：
10.1002/rcm.3289
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发表时间：
2007-01-01
影响因子：
2
通讯作者：
Puschner, Birgit
中科院分区：
文献类型：
--
作者：
Filigenzi, Michael S.;Tor, Elizabeth R.;Puschner, Birgit
2007年初，被怀疑与许多宠物死亡有关的化合物三聚氰胺被确定用于喂猪供人食用。建立了固相萃取-高效液相色谱-串联质谱法（HPLC/ MS/MS）分析猪肌肉组织中三聚氰胺的方法。用50%乙腈水溶液提取三聚氰胺。将匀浆离心，将上清液酸化并用二氯甲烷洗涤。采用混合模式C8/强阳离子交换SPE净化水提取物，然后浓缩，用稳定的同位素标记的三聚氰胺类似物强化，并通过HPLC/MS/MS进行分析。使用醚连接的苯基柱，乙酸铵/乙酸和乙腈作为移动的相进行梯度HPLC分离。采用多反应监测（MRM）模式，三聚氰胺有两个吸收子-产物离子跃迁，内标物有一个跃迁。使用溶剂中三聚氰胺浓度范围为50至2000 ng/mL的五点校准曲线来建立仪器响应。该方法进行了验证，通过分析7个重复的猪肌肉组织样品强化与10纳克/克的三聚氰胺。7次重复测定的平均回收率为83%，相对标准偏差为6.5%，计算的方法检测限为1.7 ng/g。版权所有（C）2007约翰威利父子有限公司
In early 2007 it was determined that the compound melamine, suspected of having been involved in the deaths of numerous pets, had been fed to hogs intended for human consumption. This report describes a method for the analysis of melamine in porcine muscle tissue using solid-phase extraction (SPE) and high-performance liquid chromatography/tandem mass spectrometry (HPLC/ MS/MS). Melamine was extracted in 50% acetonitrile in water. Homogenates were centrifuged and supernatants were acidified and washed with methylene chloride. The aqueous extracts were cleaned up using mixed-mode C8/strong cation exchange SPE and then concentrated, fortified with a stable isotope-labeled analog of melamine, and analyzed by HPLC/MS/MS. Gradient HPLC separation was performed using an ether-linked phenyl column with ammonium acetate/acetic acid and acetonitrile as the mobile phase. Multiple reaction monitoring (MRM) mode of two precursor-product ion transitions for melamine and one for the internal standard was used. A five point calibration curve ranging from 50 to 2000 ng/mL of melamine in solvent was used to establish instrument response. The method was validated by analysis of seven replicate porcine muscle tissue samples fortified with 10 ng/g of melamine. The mean recovery for the seven replicates was 83% with 6.5% relative standard deviation and the calculated method detection limit was 1.7 ng/g. Copyright (C) 2007 John Wiley & Sons, Ltd.