高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量 - 食品科学.pdf

228 2015, Vol.36, No.16 食品科学 ※安全检测 高效液相色谱-串联质谱法快速测定甘蔗中 杀虫双残留量 黄健祥，路大海，丁晨红，寥若昕，王富华* （广东省农业科学院农产品公共监测中心，农业部农产品质量安全检测与评价重点实验室， 农业部农产品质量安全风险评估实验室（广州），广东 广州 510640 ） 摘  要：建立了一种简便、快速、灵敏、准确的甘蔗中杀虫双的液相色谱- 串联质谱分析方法。优化了色谱、质 V V 谱条件和提取溶剂的组成，以甲醇-水（50 ∶50 ， / ）提取样品中的杀虫双，离心后上层清液过滤后直接上机检 测，无需进一步净化。甘蔗中杀虫双的检出限为1.0 μg/kg ，定量限为4.0 μg/kg 。甘蔗中5 个添加量4.0 、10、100、 200 μg/kg和500 μg/kg 的回收率为62.3%～108.4%，相对标准偏差为5.1%～14.8% 。采用本方法分析了8 例广州市场 上的甘蔗样品，均未检出杀虫双。 关键词：杀虫双；甘蔗；液相色谱- 串联质谱 Fast Detection of Bisultap Residue in Sugarcane by Liquid Chromatography-Tandem Mass Spectrometry * HUANG Jianxiang, LU Dahai, DING Chenhong, LIAO Ruoxin, WANG Fuhua (Laboratory of Quality and Safety Risk Assessment for Agro-product (Guangzhou), Ministry of Agriculture, Key Laboratory of Testing and Evaluation for Agro-product Quality and Safety, Ministry of Agriculture, Public Monitoring Center for Agro-product, Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China) Abstract: In this study, a simple, fast, sensitive and accurate liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed for the analysis of bisultap in sugarcane. The chromatographic conditions, the mass spectrometry parameters and the composition of extraction solvent were optimized. Bisultap was extracted with 50 % methanol-water V V (50:50, / ). Then, the extraction phase was filtered after centrifugation, followed by LC-MS-MS detection without further purification. The limit of detection for bisultap in sugarcane was 1.0 μg/kg and the limit of qua