Ramos M, Muñoz P, Aranda A, Rodriguez I, Diaz R, Blanca J
Unidad de Residuos Zoosanitarios, Centro Nacional de Alimentación, Agencia Española de Seguridad Alimentaria, Ctra. de Pozuelo Km 2, Majadahonda, Madrid, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Jul 5;791(1-2):31-8. doi: 10.1016/s1570-0232(03)00186-7.
A liquid chromatographic method with mass spectrometric detection and identification (LC-MS) is presented for the determination of chloramphenicol (CAP) in shrimp tissues. Homogenized shrimp samples were extracted with phosphate buffer (pH 7.0). Clean-up was carried out on a C(18) SPE cartridge. Chloramphenicol was determined by LC-MS-ESI in negative mode. The column used was a Symmetry Shield with a mixture of acetonitrile-water (25:75) as mobile phase. Shrimp samples were fortified at CAP levels between 0.2 and 50 ng g(-1) with 5D-CAP as internal standard. At these levels, accuracies lay between 101 and 110% and between-day reproducibilities were lower than 7.1%, expressed as the variation coefficient of the mean. Limit of decision (CCalpha) was 0.02 ng g(-1). Limit of quantitation (LOQ) was 0.2 ng g(-1).
本文介绍了一种采用液相色谱-质谱检测和鉴定（LC-MS）法测定虾组织中氯霉素（CAP）的方法。将虾样品匀浆后用磷酸盐缓冲液（pH 7.0）提取。采用C(18)固相萃取柱进行净化。氯霉素采用LC-MS-ESI负离子模式测定。所用色谱柱为Symmetry Shield，以乙腈-水（25:75）混合液作为流动相。虾样品以5D-CAP作为内标，在0.2至50 ng g(-1)的氯霉素添加水平下进行加标。在这些水平下，准确度在101%至110%之间，日间重现性低于7.1%（以平均值的变异系数表示）。决策限（CCalpha）为0.02 ng g(-1)。定量限（LOQ）为0.2 ng g(-1)。
