Development of Simultaneous Analytical Method for Imidazolinone Herbicides from Livestock Products by UHPLC-MSMS

Abstract

A simultaneous analytical method, which used LC/MSMS for imidazolinone herbicides from livestock products (egg, milk, beef, pork, and chicken) for monitoring, was developed with a QuEChERS preparation. A weighed sample (5 g) in a 50 mL conical tube was added to 0.1 M potassium phosphate dibasic solution (5 mL) and shaken for 10 min. After shaking, 0.5 mL of 6 N HCl and 5 mL of acetonitrile were added, and this solution was shaken for 10 min. Additionally, QuEChERS extraction salts (original method, 4 g MgSO4, 1 g NaCl) were added to the sample in a 50 mL conical tube. The mixture was strongly shaken for 1 min and centrifuged at 3000× g for 10 min. The acetonitrile layer was purified with dSPE (150 mg MgSO4, 25 mg C18) and was centrifuged at 13,000× g for 5 min. The supernatant was filtered with a membrane filter (pore size: 0.2 μm) before analysis. The ME (%, matrix effect) range for almost all analytes was −6.56 to 7.11%. MLOD (method limit of detection) and MLOQ (method limit of quantitative) values were calculated by the S/N ratio. MLOQs were 0.01 mg/kg. The linear correlation coefficients (R2) were >0.99 with the range of 0.5~25 μg/kg for all of the imidazolinone herbicides. The recoveries (of imidazolinone herbicides) were in the range of 76.1~110.6% (0.01 mg/kg level), 89.2~97.1% (0.1 mg/kg level), and 94.4~104.4% (0.5 mg/kg level). These are within the validation criteria (to recover 70–120% with RSD <20%). The method demonstrated the simple, rapid, high throughput screening and quantitative analysis of imidazolinone herbicide residues for monitoring in livestock products.

Determination of Modified QuEChERS Method for Chlorothalonil Analysis in Agricultural Products Using Gas Chromatography–Mass Spectrometry (GC-MS/MS)

“…The ionization efficiency of the target analyte can be altered by the matrix, resulting in ion suppression or enhancement, and may affect the GC-MS/MS analytical method. The matrix effect is indicated as positive or negative and is typically classified as small (−20 < ME < 20), medium (−50 < ME < −20, 20 < ME < 50), or strong (ME < −50, ME > 50) [27,28]. Except for brown rice, all food matrixes were observed to be in the ~−21.5 to −51.4% range and indicated a signal suppression effect.…”