高效液相色谱法检测猪肉中安眠酮残留量.pdfVIP

※分析检测 食品科学 2010, Vol. 31, No. 18 295 高效液相色谱法检测猪肉中安眠酮残留量 吕 飞，朱事康，黄 刚，曹维强，吴云普 (惠州出入境检验检疫局综合技术中心，广东 惠州 5 16006) 摘 要：建立高效液相色谱法(HPLC)检测猪肉中安眠酮残留量。经过实验确定用二氯甲烷提取，固相萃取(SPE) 柱净化，流动相定容后用高效液相色谱仪测定；采用乙腈:乙酸胺溶液(25mmol/L)=40 :60( V/ V)为流动相，22 6nm 为 测定波长，1.0mL/min 的流速。在0.020～0.20mg/kg 范围内具有良好的线性关系，最低检测限为0.020mg/kg ，回收 4 3 率在70% ～110% 之间，标准曲线回归方程为Y=6 .90 ×10 X +3 .7 1 ×10 ，相关系数为0 .999 。此法操作简便、快 速、灵敏、准确，样品处理简便易行，适用于测定猪肉中的安眠酮。 关键词：高效液相色谱法；猪肉；安眠酮；固相萃取 Determination of Methaqualone Residues in Pork by High Performance Liquid Chromatography . . LU F ei ，ZHU Shi-kan g ，HUANG Gang ，CAO Wei-qiang ，WU Yun-pu (Center of Comprehensive Technology, Huizhou Entry-Exit Inspection and Quarantine Bureau , Huizhou 5 16006, China) Abstract ：A high performance liquid chromatographic method was established to determine the content of methaqualone residues in pork. Sample extraction was carried out using dichloromethane as the extraction solvent, followed by clean-up on a solid-phase extraction column and dillution to a certain volum with the mobile phase composed of acetonitrile and 25 mmol/L ammonium acetate before inj ection onto HPLC system. The detection wavelength was 226 nm and the mobile phase flow rate 4 3 was 1.0 mL/min. The calibration curve of the developed method was as follows: Y = 6.90 ×10 X +3.7 1 ×10 , with a correlation coefficient of 0.999, which exhibited good linearity over the concentration range from 0.020 to 0.20 mg/kg. The detection limit was 0.020 mg/kg, and the inter- and intra-laboratory average spi