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

Determination of carbendazim and thiophanate-methyl in red wine by high pressure liquid chromatography-linear ion trap mass spectrometry

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、50μg/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0.063μg/L和0.019μg/L,定量限(LOQs)分别为0.125μg/L和0.075μg/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, 20μg/L and 50μg/L were 82.5%~103.1%and 93.7%~115.2%, respectively. The limits of detection (LODs) were 0.063 μg/L and 0.019μg/L, and the limits of quantification (LOQs) were 0.125μg/L and 0.075μg/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.