Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China.
Anal Bioanal Chem. 2011 Aug;401(3):1051-8. doi: 10.1007/s00216-011-5148-3. Epub 2011 Jun 10.
The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 μg kg(-1), while the limit of quantification did not exceed 2 μg kg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.
采用 QuEChERS 前处理方法，结合超高效液相色谱-串联质谱法（UPLC-MS/MS），建立了同时测定果蔬中二酰肼类杀虫剂残留的分析方法。采用乙腈提取 6 种果蔬基质中的 4 种杀虫剂（丁醚脲、甲氧虫酰肼、氯虫苯甲酰胺和氟苯虫酰胺），然后用 PSA 或 C18 作为吸附剂净化，再进行 UPLC-MS/MS 分析。采用电喷雾离子源（ESI+）正离子模式测定丁醚脲、甲氧虫酰肼和氟苯虫酰胺，ESI-负离子模式测定氯虫苯甲酰胺，目标化合物在 3.0 min 内可完全分离。在不同基质中，4 种目标化合物的检出限均低于 0.6 μg kg(-1)，定量限均不超过 2 μg kg(-1)。采用 PSA 和 C18 两种吸附剂的 QuEChERS 方法，结合基质匹配标准品，在 4 个添加水平（0.01、0.05、0.1 和 1 mg kg(-1)）下，不同基质中的回收率和相对标准偏差（RSD）均令人满意。该方法在苹果、葡萄、黄瓜、番茄、白菜和菠菜中的平均回收率为 74.2%-112.5%，相对标准偏差为 1.4%-13.8%（n = 5）。本研究为我国制定蔬菜和水果中二酰肼类杀虫剂的最大残留限量和分析方法提供了理论依据。
