Jiménez A M, López de Cerain A, Gonzalez-Peñas E, Bello J
Department of Food Science and Toxicology, Faculty of Pharmacy, University of Navarra, Pamplona, Spain.
Food Addit Contam. 2001 Jun;18(6):559-63. doi: 10.1080/02652030117035.
A solid phase extraction procedure followed by HPLC analysis with fluorescence detection has been developed for ochratoxin A (OTA) in pâtés derived from pig liver. After a previous extraction of OTA with 60% acetonitrile, all the samples were purified through C8 columns. The percentage recovery was 85.7% and the lower limits calculated for accurate detection and quantitation were 0.56 ng/g and 0.84 ng/g respectively. The HPLC procedure showed a good linearity in the interval of equivalent OTA concentrations of 0.84 to 3 ng/g. Values <10% were obtained for precision in HPLC determinations performed (n = 3) and (n = 9). Stability of calibration standards and samples during the analytical procedure was also demonstrated. This method was successfully applied to 38 pig-derived pâtés and three samples were found to be positive with OTA levels above the detection limit. The highest concentration (1.77 ng/g) has been found in a home-made pâté.
已开发出一种固相萃取方法，随后进行带荧光检测的高效液相色谱分析，用于检测猪肝制成的肉酱中的赭曲霉毒素A（OTA）。在用60%乙腈预先萃取OTA后，所有样品通过C8柱进行纯化。回收率为85.7%，准确检测和定量的下限分别为0.56 ng/g和0.84 ng/g。高效液相色谱法在0.84至3 ng/g的等效OTA浓度区间内显示出良好的线性。在进行的高效液相色谱测定（n = 3）和（n = 9）中，精密度值<10%。还证明了校准标准品和样品在分析过程中的稳定性。该方法成功应用于38种猪源肉酱，发现3个样品OTA呈阳性，含量高于检测限。在一份自制肉酱中发现了最高浓度（1.77 ng/g）。
