固相萃取高效液相色谱法测定辣椒油中苏丹红和对位红染料.PDF

※分析检测 食品科学 2009, Vol. 30, No. 16 243 1 1 1 1 2 吴银良 ，杨 挺 ，赵 健 ，皇甫伟国 ，沈建忠 (1.农业部农产品质量安全监督检验测试中心(宁波) ，浙江宁波 315040 ；2. 中国农业大学动物医学院，北京 100193) 建立辣椒油中苏丹红和对位红染料的固相萃取- 高效液相色谱分析方法。样品经乙腈提取，提取液加水混 匀后过C18 固相萃取(SPE)柱净化，正已烷洗脱，洗脱液经旋转浓缩蒸干后用甲醇溶解进行高效液相色谱梯度洗脱分 析，外标法定量。检出限为7～7.2 μg/kg 。在添加浓度25～250 μg/kg 范围内，平均添加回收率在78.3%～93.5% 范 围内，日内变异系数在3.3%～9.2% 之间，日间变异系数在4.6% ～10.6% 之间。各染料峰面积与样品浓度在15～ 2000 μg/L 范围内呈良好的线性关系，线性回归系数大于0.9997 。 高效液相色谱；固相萃取；苏丹红；对位红 Solid-phase Extraction and HPLC Determination of Six Sudan Reds and Para Red in Pepper Oil 1 1 1 1 2 WU Yin-liang ，YANG Ting ，ZHAO Jian ，HUANGFU Wei-guo ，SHEN Jian-zhong (1. The Supervision, Inspection and Testing Center of Agricultural Products Quality and Security，Ministry of Agriculture, Ningbo, Ningbo 315040, China；2. College of Veterinary Medicine, China Agricultural University, Beijing 100193, China) Abstract：A method was presented for determining six Sudan reds and Para red in pepper oil using solid-phase extraction (SPE) and HPLC. Samples were extracted with acetonitrile and cleaned up on a C18 SPE column using n-hexane as the eluant, and the eluate was evaporated to dryness and dissolved in methanol prior to HPLC analysis. The analytes were detected at 510 nm, and quantified using an external calibration method. The detection limits were 7.0－7.2 μg/kg for six Sudan reds and Para red in pepper oil. At three spiked levels of 25 －250 μg/kg, the average recoveries for six Sudan reds and Para red in pepper oil were 78.3% －93.5%, and the intra and inter CVs were 3.3% －9.2% and 4.6% －10.6%, respectively. There was a good linear correlation (r ＞ 0. 9997) between the pe