高压液相色谱-线性离子阱串联质谱法测定红葡萄酒中多菌灵和甲基硫菌灵
目的 建立红葡萄酒中多菌灵和甲基硫菌灵残留的高压液相色谱-串联线性离子阱质谱(HPLC-LIT-MS/MS)检测方法。方法 样品经过乙腈提取, 在梯度洗脱程序下经CAPCELL PAK CR 1:20色谱柱分离后, 采用HPLC-LIT-MS/MS, 在二级质谱选择反应监测(SRM)模式进行测定。结果 红葡萄酒中多菌灵和甲基硫菌灵添加水平为10、20、50 μg/L时, 平均回收率分别为82.5%~103.1%和93.7%~115.2%。检出限(LODs)分别为0.063 μg/L和0.019 μg/L, 定量限(LOQs)分别为0.125 μg/L和0.075 μg/L。结论 该方法快速简便, 灵敏度高, 准确度和精密度均满足痕量分析要求。
Objective To develop a method of high pressure liquid chromatography-linear ion trap mass spectrometry (HPLC-LIT-MS) for the determination of carbendazim and thiophanate-methyl in red wine. Methods Samples were ultrasonically extracted with acetonitrile, separated on a CAPCELL PAK CR 1:20 column with gradient elution and the mass spectrometric acquisition was carried out under the mode of selected reaction monitoring (SRM). Results The average recoveries of carbendazim and thiophanate-methyl in red wine at 10, 20 μg/L and 50 μg/L were 82.5%~103.1% and 93.7%~115.2%, respectively. The limits of detection (LODs) were 0.063 μg/L and 0.019 μg/L, and the limits of quantification (LOQs) were 0.125 μg/L and 0.075 μg/L. Conclusion The established method is fast, simple, selective, precise and accurate, and it is suitable for quantitative and qualitative detection of carbendazim and thiophanate-methyl in red wine.
标题:高压液相色谱-线性离子阱串联质谱法测定红葡萄酒中多菌灵和甲基硫菌灵
英文标题:Determination of carbendazim and thiophanate-methyl in red wine by high pressure liquid chromatography-linear ion trap mass spectrometry
作者:
李鹏 国家食品安全风险评估中心
刘凯丽 北京市丰台区动物卫生监督所
杨欣 国家食品安全风险评估中心
赵云峰 国家食品安全风险评估中心;卫生部食品安全风险评估重点实验室
吴永宁 国家食品安全风险评估中心;卫生部食品安全风险评估重点实验室
中文关键词:高压液相色谱-线性离子阱质谱法(HPLC-LIT-MS),红葡萄酒,多菌灵,甲基硫菌灵,
英文关键词:high pressure liquid chromatography-linear ion trap mass spectrometry (HPLC-LIT-MS),red wine,carbendazim,thiophanate-methyl,
发表日期:2012-11-08
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