Tsartsali Niki, Samanidou Victoria F
Department of Chemistry, Laboratory of Analytical Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
Anal Chem Insights. 2015 Dec 20;10:53-8. doi: 10.4137/ACI.S31727. eCollection 2015.
A quick, easy, cheap, effective, rugged, and safe (QuEChERS) dispersive extraction method is proposed herein for the isolation and cleanup of melamine and cyromazine from chicken egg yolk. Analytes are determined by high-performance liquid chromatography using photodiode array detector after separation on a LiChroCART® (250 × 4 mm)-LiChrospher® RP-8e, 5 μm analytical column using a mobile phase of 0.1% trifluoracetic acid and methanol (80:20 v/v) delivered isocratically at a flow rate of 1 mL/minute. Extraction of isolated compounds was achieved by methanol and acetonitrile mixture (1:1 v/v). Recovery rates ranged between 74.5% and 115.8%. The method was validated in terms of 657/2002/EC decision. The within-laboratory reproducibility, expressed as a relative standard deviation, was <11%. Decision limits (CCalfa) were 2.56 mg/kg for melamine and 0.22 mg/kg(-1) for cyromazine, and the corresponding results for detection capability (CCbeta) were 2.8 mg/kg for melamine and 0.24 mg/kg for cyromazine. Ruggedness was estimated according to the Youden approach studying egg yolk mass, sorbent mass, centrifugation time, organic solvents volume, evaporation temperature, and vortex time.
本文提出了一种快速、简便、廉价、高效、耐用且安全的（QuEChERS）分散萃取方法，用于从鸡蛋蛋黄中分离和净化三聚氰胺和环丙氨嗪。使用光电二极管阵列检测器的高效液相色谱法对分析物进行测定，分离在LiChroCART®（250×4 mm）-LiChrospher® RP-8e、5μm分析柱上进行，流动相为0.1%三氟乙酸和甲醇（80:20 v/v），等度洗脱，流速为1 mL/分钟。通过甲醇和乙腈混合物（1:1 v/v）实现对分离化合物的萃取。回收率在74.5%至115.8%之间。该方法根据657/2002/EC决议进行了验证。以相对标准偏差表示的实验室内重现性<11%。三聚氰胺的决策限（CCalfa）为2.56 mg/kg，环丙氨嗪的决策限为0.22 mg/kg（-1），三聚氰胺的相应检测能力（CCbeta）结果为2.8 mg/kg，环丙氨嗪为0.24 mg/kg。根据尤登方法评估耐用性，研究蛋黄质量、吸附剂质量、离心时间、有机溶剂体积、蒸发温度和涡旋时间。
