State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China.
J Chromatogr A. 2013 Jul 19;1299:71-7. doi: 10.1016/j.chroma.2013.05.049. Epub 2013 May 27.
A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for the simultaneous determination of spirotetramat and its four metabolites in fruits (apple, peach) and vegetables (cabbage, tomato, potato, cucumber), based on the use of liquid extraction/partition and dispersive solid phase extraction (dispersive-SPE) followed by ultrahigh-performance chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS), was established. Acidified acetonitrile (containing 1% (v/v) acetic acid) as the extraction solvent and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate (NaOAc). The extract was then cleaned up by dispersive-SPE using graphitized carbon black (GCB) as selective sorbent. Further optimization of sample preparation and determination achieved recoveries of between 82 and 110% for all analytes with RSD values lower than 14% in apple, peach, cabbage, tomato, potato and cucumber at three levels (10, 100 and 1000μg/kg). The method showed excellent linearity (R(2)≥0.9895) for all studied analytes. The determination of the target compounds was achieved in less than 6.0min using an electrospray ionization source in positive mode (ESI+). The method is demonstrated to be convenient and reliable for the routine monitoring of spirotetramat and its metabolites in fruits and vegetables.
基于液液萃取/分配和分散固相萃取（dispersive-SPE），同时使用超高效液相色谱-串联质谱（UHPLC-MS/MS），建立了一种改良的快速、简便、廉价、有效、坚固、安全（QuEChERS）方法，用于同时测定水果（苹果、桃）和蔬菜（白菜、番茄、土豆、黄瓜）中螺虫乙酯及其四种代谢物。酸化乙腈（含 1%（v/v）乙酸）作为提取溶剂，同时通过添加无水硫酸镁（MgSO4）和无水乙酸钠（NaOAc）形成液-液分配。然后，通过使用石墨化炭黑（GCB）作为选择性吸附剂进行分散固相萃取净化提取物。通过进一步优化样品制备和测定，在苹果、桃、白菜、番茄、土豆和黄瓜中，所有分析物的回收率在 82%至 110%之间，相对标准偏差（RSD）低于 14%，在三个水平（10、100 和 1000μg/kg）下。该方法对所有研究分析物均表现出良好的线性（R²≥0.9895）。使用电喷雾电离源在正模式（ESI+）下，所有目标化合物的测定时间均少于 6.0min。该方法被证明可用于水果和蔬菜中螺虫乙酯及其代谢物的常规监测，简便可靠。
