title: Rapid Multi-Residue Analysis of Pesticides in Pulses by LC-MS/MS.
abstract: Rapid multi-residue analysis of pesticides in pulses was developed using LC-MS/MS. Pesticide residues in 5 g of homogenized pulses were extracted with 30 mL of acetonitrile and salted out with 4 g of anhydrous magnesium sulfate and 2 g of sodium chloride in the presence of citrate buffer in a disposable tube. The resulting residues were extracted with 30 mL of acetonitrile, and co-extractives were removed on a handmade four-layer column, consisting of a layer of Z-Sep/C18 (20 mg/50 mg) dry particles on top of a three-layer, custom-made (pre-packed) column (lower bed: 60 mg of PSA, middle bed: 30 mg of GC, and top bed: 60 mg of C18) packed in a 10 mm internal diameter polypropylene column (3 mL). The developed method showed good recoveries of pesticides in soybean, lentil, white kidney bean and garbanzo. According to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan, recovery tests were conducted in soybeans fortified with 107 kinds of pesticides at the levels of 0.01 and 0.1 μg/g, respectively. At each concentration 2 samples were extracted on 5 separate days. Pesticides in the test solution were determined by LC-MS/MS using scheduled MRM. As regards the trueness of this method for 107 pesticides in soybeans, 97 pesticides were in the range of 70-120% with satisfactory repeatability and within-run reproducibility. This new method is expected to be applicable for routine examination of pesticide residues in soybeans.
authors: Tokyo Metropolitan Institute of Public Health.
authors: Keiko
authors: K
authors: Iwakoshi
authors: Kenji
authors: K
authors: Otsuka
authors: Yasuhiro
authors: Y
authors: Tamura
authors: Sanae
authors: S
authors: Tomizawa
authors: Tamako
authors: T
authors: Masubuchi
authors: Yumiko
authors: Y
authors: Yamaki
authors: Yukiko
authors: Y
authors: Nakagawa
authors: Ryoko
authors: R
authors: Masuda
authors: Shota
authors: S
authors: Suto
authors: Yoshie
authors: Y
authors: Kokaji
authors: Tetsuya
authors: T
authors: Shindo
authors: Ichiro
authors: I
authors: Takano
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D029863:Cicer / Q000737:chemistry*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D027806:Lens Plant / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D027805:Phaseolus / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods; D013025:Glycine max / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D010573:Pesticide Residues