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J.Health Sci., 50(1), 17-24, 2004
Simultaneous Determination of Emamectin, its Metabolites, Milbemectin, Ivermectin and
Abamectin in Tomato, Japanese Radish
and Tea by LC/MS
Kimihiko Yoshii,*, a Susumu
Ishimitsu,a Yasuhide
Tonogai,a Kiyomi
Arakawa,b
Hideaki Murata,b and Hirohisa
Mikamib
aOsaka Branch, National Institute of Health Sciences, 1-1-43, Hoenzaka, Chuo-ku, Osaka 540-0006, Japan and
bAnalytical Application Department, Shimadzu Corporation, 1, Nishinokyo-Kuwabaracho, Nakagyo-ku, Kyoto 604-8511, Japan
We developed a simple and rapid analytical method for determining the residues of emamectin benzoate,
milbemectin, abamectin, ivermectin and emamectin metabolites in tomato, Japanese Radish and Japanese tea by
liquid chromatography/mass spectrometer (LC/MS) with electrospray ionization (ESI). A sample extracted with
acetone was simply cleaned up using only a Sep-Pak C18, and then directly measured by LC/MS (ESI). Several
LC/MS measurement conditions were studied that included the mobile phase, solvent for sample solution, range
of calibration and standard deviation of the measurement. Detecting target macrocyclic lactone chemicals with
methanol as the mobile phase was more sensitive than acetonitrile, especially, milbemectin. The detection limits
of these chemicals were 0.1 to 0.5 ng/ml
(10 mu l injection), and they were similar or more sensitive to the previous
fluorescence detection method. For the measurement of these chemicals in tomato, Japanese radish and tea by
LC/MS (ESI), ion suppression was always observed. To compensate for such an effect, we used a matrix-matched
calibration. This compensation method is effective for obtaining accurate values. The recoveries by the
developed method were in an acceptable range for the screening method and 90.1-120.9% except for milbemectin
and abamectin from tea leaves that had interfering peaks.
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