State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control, MOA Key Laboratory for Pesticide Residue Detection, Zhejiang Academy of Agricultural Sciences, Hangzhou, China.
Anal Bioanal Chem. 2012 Mar;402(7):2451-62. doi: 10.1007/s00216-011-5699-3. Epub 2012 Jan 20.
A new sensitive multiresidue liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical method for the determination of 16 insect growth regulator (IGR) residues-RH-5849 (1,2-dibenzoyl-1-tert-butylhydrazine), halofenozide, methoxyfenozide, chromafenozide, fufenozide, tebufenozide, diflubenzuron, chlorbenzuron, triflumuron, hexaflumuron, novaluron, lufenuron, teflubenzuron, flucycloxuron, flufenoxuron, and chlorfluazuron-in herbs (Perilla frutescens, flos chrysanthemi, lily bulbs, and ginger) has been developed. After the herbs had been extracted with acetonitrile, a combined graphitized nonporous carbon/aminopropyl (ENVI-Carb/LC-NH(2)) cartridge and a Florisil cartridge were used to clean up the extracts. LC-MS/MS was performed in multiple reaction monitoring mode with two specific precursor ion-product ion transitions per IGR to confirm and quantitate the residues in herbs. Quantitation was performed on the basis of matrix-matched calibrations. The method showed excellent linearity (r(2) > 0.99) and precision (relative standard deviations of 13.6 or lower) for all the target insecticides. The limits of quantitation were 0.6-10 μg kg(-1) for the 16 insecticides in the four herbs. The average recoveries, measured at three concentrations (0.01, 0.1, 1 mg kg(-1)), were in the range 74.8-105.3%. The method was satisfactorily applied for the analysis of 60 herb samples (Perilla frutescens, flos chrysanthemi, lily bulbs, and ginger). Hexaflumuron was detected at concentrations of 0.029 and 0.051 mg kg(-1) in Perilla frutescens.
一种新的灵敏多残留液相色谱-串联质谱（LC-MS/MS）分析方法用于测定 16 种昆虫生长调节剂（IGR）残留- RH-5849（1,2-二苯甲酰基-1-叔丁基肼）、氟虫腈、甲氧虫酰肼、环虫酰肼、虱螨脲、虫酰肼、除虫脲、氯苯脲、三氟脲、噻嗪酮、除虫脲、氟铃脲、氟虫脲、氟环脲、氟虫脲和氯氟脲-在草药（紫苏、菊花、百合鳞茎和生姜）中。草药用乙腈提取后，用石墨化非多孔碳/氨丙基（ENVI-Carb/LC-NH2）和 Florisil 小柱进行净化。LC-MS/MS 采用多反应监测模式，每个 IGR 有两个特定的前体离子-产物离子转换，以确认和定量草药中的残留。定量是基于基质匹配校准进行的。该方法对所有目标杀虫剂均表现出良好的线性（r(2)＞0.99）和精密度（相对标准偏差为 13.6 或更低）。在四种草药中，16 种杀虫剂的定量限为 0.6-10 μg kg(-1)。在三个浓度（0.01、0.1、1 mg kg(-1))下测量的平均回收率在 74.8-105.3%之间。该方法满意地应用于 60 种草药样品（紫苏、菊花、百合鳞茎和生姜）的分析。在紫苏中检测到噻嗪酮的浓度为 0.029 和 0.051 mg kg(-1)。
