QuEChERS-高效液相色谱-串联质谱法测定植物源性食品中噻氟隆和炔草隆残留

Determination of Thiazafluron and Buturon in Vegetative Foods by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了QuEChERS前处理-高效液相色谱-串联质谱法(HPLC-MS/MS)同时检测植物源性食品中噻氟隆和炔草隆残留的分析方法。样品以酸化乙腈提取,经石墨化碳黑(GCB)净化。采用C18色谱柱进行分离,以甲醇-0.1%甲酸溶液(含5mmol/mL乙酸铵)为流动相,梯度洗脱。质谱采用电喷雾正离子电离(ESI+),多重反应监测模式(MRM)检测。以保留时间和特征离子对进行定性,基质匹配外标法定量。结果表明:在葡萄、葡萄干、西红柿、大米、苹果、枸杞、黄瓜、小麦粉、白菜9种基质中,噻氟隆和炔草隆在各自线性范围内线性关系良好(相关系数r2均大于0.997);噻氟隆和炔草隆的定量限(S/N=10)分别为0.4、1.0μg/kg,在3个加标水平(1、2、10倍定量限)下,噻氟隆的回收率为84.7%~107.7%,相对标准偏差为4.2%~16.3%;炔草隆的回收率为74.7%~110.0%,相对标准偏差为4.3%~12.8%。该方法简单、快速、准确、灵敏、安全,适用于植物源性食品中噻氟隆和炔草隆残留的快速确证和定量分析。

A method was developed for the simultaneous determination of thiazafluron and buturon in vegetative foods by QuEChERS-high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The sample was extracted with acidic acetonitrile,and then cleaned up by GCB.The analytes were separated on a C18 column with gradient elution of methanol and 0.1% formic acid in water（including 5 mmol/mL ammonium acetate）at a flow rate of 0.25mL/min.The mass spectrometer was carried out with electrospray positive ion source（ESI＋）,and multiple reaction monitoring mode（MRM）.The qualitative analysis was based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions,and the quantitative analysis was carried out by matrix-matched external standard method.The results showed that calibration curves had good linearity for thiazafluron and buturon,and the correlation coefficients（r）were larger than 0.997;the limit of quantification（LOQ,S/N=10）of thiazafluron in nine different matrix was 0.4μg/kg,and the LOQ of buturon was 1.0μg/kg;When we spiked three levels of 1×LOQ,2×LOQ and 10×LOQ in samples,the recoveries of thiazafluron were from 84.7%to 107.7% with the RSDs from 4.2%to 16.3%,and the recoveries of buturon were from 74.7%to 110.0% with the RSDs from 4.3%to 12.8%,respectively.The method is simple,accurate,rapid,safe and sensitive,and can be used for the rapid and quantitative analysis of the residue of thiazafluron and buturon in vegetable foods.