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液相色谱-串联质谱法快速测定牛奶中的生长促进剂

Rapid multi-method for the determination of growth promoters in bovine milk by liquid chromatography-tandem mass spectrometry.

机构信息

Veterinary Laboratory of Serres, Terma Omonoias, 62110 Serres, Greece.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jul 1;930:22-9. doi: 10.1016/j.jchromb.2013.04.013. Epub 2013 Apr 18.

Abstract

A rapid multi-method was developed for the determination of 21 growth promoters from different classes, including gestagens, corticosteroids, RALs, stilbenes, steroids in bovine milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS). All compounds were eluted from the analytical column in less than 8.5min and were subsequently analyzed with atmospheric pressure chemical ionization (APCI) using both positive and negative mode. Sample preparation included extraction of the compounds with acetonitrile and purification with solid-phase extraction (SPE). The method was validated according to Commission Decision 2002/657/EC, at a validation level of 1ng/ml. The specificity, accuracy, precision, decision limit (CCα) and the detection capability (CCβ) were satisfactory evaluated. The recoveries ranged from 80.7% to 118.8% and reproducibility represented as coefficient of variance (CV) was from 1.8% to 13.0%. The CCα and CCβ values were in the ranges 0.06-0.10ng/ml and 0.11-0.17ng/ml, respectively. The developed method was applied in real samples proving its rapidness and sensitivity for the determination of the 21 growth promoters.

摘要

建立了一种快速的多方法,用于通过液相色谱-串联质谱法(LC-MS/MS)测定牛奶中的 21 种来自不同类别的生长促进剂,包括孕激素、皮质甾类、RALs、苯乙烯、甾体。所有化合物都在 8.5 分钟内从分析柱洗脱,并随后使用大气压化学电离(APCI)在正、负模式下进行分析。样品制备包括用乙腈提取化合物并通过固相萃取(SPE)进行纯化。该方法根据委员会 2002/657/EC 号决定在 1ng/ml 的验证水平上进行了验证。特异性、准确性、精密度、决策限(CCα)和检测能力(CCβ)均得到了满意的评估。回收率范围为 80.7%至 118.8%,重现性表示为变异系数(CV)为 1.8%至 13.0%。CCα和 CCβ值分别在 0.06-0.10ng/ml 和 0.11-0.17ng/ml 范围内。所开发的方法已应用于实际样品,证明其对 21 种生长促进剂的测定具有快速性和灵敏度。

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