Simple and Rapid Determination of Cypermethrin and Fenvalerate Residues in Kampo Products by Gas Chromatography-Mass Spectrometry with Negative Chemical Ionization

Abstract

In Japan, crude drugs that are used as ingredients of kampo formulae are mainly imported from China. In China, cypermethrin and fenvalerate, which are pyrethroid pesticides, are detected frequently in food exported to Japan. In fact, cypermethrin and fenvalerate have been detected in crude drugs distributed in Japan. There is concern that cypermethrin and fenvalerate will move from crude drugs to kampo products. Cypermethrin and fenvalerate in kampo products are controlled by a self-imposed residual pesticide limit set by the Japan Kampo Medicine Manufacturers Association. Several methods to analyze cypermethrin and fenvalerate in kampo products have been reported, but they are time-consuming, require expensive column clean-up, and use large amounts of organic solvents. In this study, a simple, rapid, and inexpensive sample preparation method was developed to determine cypermethrin and fenvalerate levels in kampo products by gas chromatography (GC)-mass spectrometry (MS) with negative chemical ionization (NCI). Twenty-two samples of kampo products were analyzed according to the proposed method. No samples were contaminated by cypermethrin and fenvalerate levels greater than the detection limit.

Photodegradation study of the fenvalerate insecticide by 1H NMR, 13C NMR, and GC-MS and structural elucidation of its transformation products

“…The solar light simulator was used to follow the kinetics of fenvalerate photodegradation and photoproducts formation in CH3CN by GC-MS. At t = 0, we observed two peaks of retention times tR = 28.06 and 28.28 min. These peaks corresponded to two of the four fenvalerate isomers as observed by Tagami et al (2009), who determined fenvalerate residues in kampo products by GC-MS with negative chemical ionization. 31 Solar light simulator irradiation of fenvalerate in CH3CN led to the degradation of both fenvalerate isomer peaks and to the appearance of new, different peaks.…”

Simultaneous determination of cypermethrin and fenvalerate residues in tomato by gas chromatography and their applications to kinetic studies after field treatment

“…The improper use of cypermethrin and fenvalerate can generate a considerable amount of residue, higher than the MRL, 0.03-0.5 mg/g, as established by the Brazilian Sanitary Surveillance Agency (ANVISA, 2009), as well as other regulatory agencies such as the Codex Alimentarius (FAO/WHO, 2009), which is from 0.3 to 0.5 mg/g. Pyrethroid residues have been determined using chromatographic techniques with various detectors such GC-ECD (De Pinho et al, 2010;Chen et al, 2011;Sandra et al, 2005;Su et al, 2007), GC-FID, GC-MS (Beltran et al, 2003;Tagami et al, 2009;Albero et al, 2004;Kazuaki et al, 1997), HPLC-UV (Metwally et al, 1997) and HPLC-MS (Klein and Alder, 2003), in various samples of vegetables and fruits. Thus far, there have been no reports in the literature of simultaneous determination of cypermethrin and fenvalerate in tomato.…”

“…Pyrethroid residues have been determined using chromatographic techniques with various detectors such GC‐ECD (De Pinho et al , ; Chen et al , ; Sandra et al , ; Su et al , ), GC‐FID, GC‐MS (Beltran et al , ; Tagami et al , ; Albero et al , ; Kazuaki et al , ), HPLC‐UV (Metwally et al , ) and HPLC‐MS (Klein and Alder, ), in various samples of vegetables and fruits. Thus far, there have been no reports in the literature of simultaneous determination of cypermethrin and fenvalerate in tomato.…”

Simple and Rapid Determination of Organochlorine Pesticide Residues in Kampo Products by Gas Chromatography/Mass Spectrometry with Negative Chemical Ionization

“…Sample preparation method was based on the previous report. 7) When the recovery test was conducted according to the previous report, 7) a matrix enhancement effect was observed. So the sample preparation method was slightly changed and sulfuric treatment of the extraction liquid was supplemented.…”

“…6) Furthermore, a simple and rapid determination of pyrethroid pesticides in kampo products by GC/MS with NCI was also reported. 7) In this study, a simple, rapid, and inexpensive sample preparation method to determine BHCs and DDTs in kampo products was investigated using GC/MS with NCI.…”