Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi)
Online ISSN : 1882-1006
Print ISSN : 0015-6426
ISSN-L : 0015-6426
Volume 52, Issue 4
Displaying 1-8 of 8 articles from this issue
Review
Original Papers
  • Hisako SAKUMA, Yoichi KAMATA, Yoshiko SUGITA-KONISHI, Hiroshi KAWAKAMI
    2011 Volume 52 Issue 4 Pages 220-225
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    A rapid, sensitive convenient method for determination of aflatoxin M1 (AFM1) in cheese and butter by HPLC was developed and validated. The method employs a safe extraction solution (mixture of acetonitrile, methanol and water) and an immunoaffinity column (IAC) for clean-up. Compared with the widely used method employing chloroform and a Florisil column, the IAC method has a short analytical time and there are no interference peaks. The limits of quantification (LOQ) of the IAC method were 0.12 and 0.14 μg/kg, while those of the Florisil column method were 0.47 and 0.23 μg/kg in cheese and buffer, respectively. The recovery and relative standard deviation (RSD) for cheese (spiked at 0.5 μg/kg) in the IAC method were 92% and 7%, respectively, while for the Florisil column method the corresponding values were 76% and 10%. The recovery and RSD for butter (spiked at 0.5 μg/kg) in the IAC method were 97% and 9%, and those in the Florisil method were 74% and 9%, respectively. In the IAC method, the values of in-house precision (n=2, day=5) of cheese and butter (spiked at 0.5 μg/kg) were 9% and 13%, respectively. The IAC method is superior to the Florisil column method in terms of safety, ease of handling, sensitivity and reliability. A survey of AFM1 contamination in imported cheese and butter in Japan was conducted by the IAC method. AFM1 was not detected in 60 samples of cheese and 30 samples of butter.
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  • Maki KOBAYASHI, Kenji OTSUKA, Yasuhiro TAMURA, Sanae TOMIZAWA, Kyoko K ...
    2011 Volume 52 Issue 4 Pages 226-236
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    A simple and rapid method using GC-MS and GC-FPD for the determination of pesticide contamination in processed food has been developed. Pesticides were extracted from a sample with ethyl acetate in the presence of anhydrous sodium sulfate, then cleaned up with a combination of mini-columns, such as macroporous diatomaceous earth, C18, GCB (graphite carbon black) and PSA. Recovery tests of 57 pesticides (known to be toxic or harmful) from ten kinds of processed foods (butter, cheese, corned beef, dried shrimp, frozen Chinese dumplings, grilled eels, instant noodles, kimchi, retort-packed curry and wine) were performed, and the recovery rates were mostly between 70% and 120%. This method can be used to judge whether or not processed foods are contaminated with pesticides at potentially harmful levels.
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  • Shizuka SAITO, Satoru NEMOTO, Rieko MATSUDA
    2011 Volume 52 Issue 4 Pages 237-243
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    A sensitive and selective analytical method for the determination of pindone in agricultural products by LC-MS/MS was developed. Pindone was extracted with acetone, and an aliquot of the crude extract was re-extracted with hexane. For lipid-rich samples, the crude extract was further cleaned up by acetonitrile-hexane partitioning. The extract was cleaned up on a tandem graphitized carbon-silica gel column. For brown rice, soybean, and tea, PSA column cleanup was added prior to LC-MS/MS determination. Average recoveries of pindone from brown rice, soybean, potato, spinach, cabbage, apple, orange, tomato, cucumber, and tea fortified at 0.001 mg/kg were 81-93%, and the relative standard deviations were 2-7%. The limit of quantitation (S/N≥10) of the developed method was 0.001 mg/kg for all the tested agricultural products.
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  • Shizuka SAITO, Takatoshi SAKAI, Satoru NEMOTO, Rieko MATSUDA
    2011 Volume 52 Issue 4 Pages 244-250
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    A sensitive and selective method for the determination of 4-hydroxycoumarin-type rodenticides (warfarin, coumatetralyl, bromadiolone, and brodifacoum) in animal products, fishery products, and honey was developed. 4-Hydroxycoumarin rodenticides were extracted with acidified acetone, and the crude extract was purified by liquid-liquid partitioning followed by PSA column cleanup. Gradient liquid chromatographic separation was performed by using an Inertsil ODS-4 column, with methanol and water containing ammonium acetate as the mobile phase. Detection was carried out on a tandem mass spectrometer with electrospray ionization in the negative mode. Average recoveries from bovine muscle, bovine liver, bovine fat, swine muscle, salmon, eel, freshwater clam, egg, milk, and honey spiked at 0.0005-0.001 mg/kg were in the range of 79-108%, and the relative standard deviations were 2-8%. The limits of quantitations of the developed method were 0.0005 mg/kg for brodifacoum, 0.001 mg/kg for warfarin, coumatetralyl, and bromadiolone.
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Note
  • Haruka OHNO, Eiji UENO, Minae WATANABE, Harumi OSHIMA, Eiichi MIKAMI
    2011 Volume 52 Issue 4 Pages 251-257
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    A multiresidue method using dual-injection, dual-column, and dual-micro electron capture detection gas chromatography (dual-column GC-μECD) was developed for the determination of PCB, organochlorine pesticides and chlordanes in marine products. The sample was extracted with hexane-acetone (2 : 1), and the extract was cleaned up by gel permeation chromatography(GPC)/solid-phase extraction (SPE). The GPC fraction was selectively collected, and loaded directly onto a graphitized carbon/PSA 2-layered column. After fractionation by 4% hydrated silica-gel column chromatography, each fraction was determined by dual-column GC-μECD. Recoveries of PCB, organochlorine pesticides and chlordanes were in the ranges of 84-109% (RSD≤21.6%), 74-117% (RSD≤14.6%) and 69-114% (RSD≤12.9%), respectively. This method is superior to single chromatography for the determination of total PCB, and should be useful for monitoring of these pollutants in marine products.
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Report
  • Atsuko TADA, Kyoko ISHIZUKI, Akio KOYAMA, Toshio FUKAI, Takumi AKIYAMA ...
    2011 Volume 52 Issue 4 Pages 258-264
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    Mulberry bark extract, a natural food additive, is described as a “root bark extract from Morus bombycis” (Japanese name: Yamaguwa) in the Notice (1996) relating to existing food additives used in Japan. The results of analyses by LC/UV and LC/MS suggested that the Mulberry bark extract products that were tested were actually made from the root bark of Morus alba (Japanese name: Maguwa) or its hybrid species, because the compositions of the constituents in the products are more similar to those in the extracts of the dried root bark of M. alba and hybrid species that are cultivated in Japan than to those of M. bombycis. In addition, the constituents of the food additive products were different from those of the natural medicine Mori Cortex products (‘Souhakuhi' in Japanese) made from the root bark of mulberry grown in China, and which is described as being derived from M. alba in the Japanese pharmacopoeia. These results were also corroborated by Principal Component Analysis using the peak areas of LC/MS analysis as explanatory variables. After this study, it was decided that Mulberry bark extract is one of the existing food additives that should be excluded from the list this year in Japan.
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Validation Study
  • Reona TAKABATAKE, Tomohiro KOIWA, Masaki KASAHARA, Kaori TAKASHIMA, Sa ...
    2011 Volume 52 Issue 4 Pages 265-269
    Published: August 25, 2011
    Released on J-STAGE: August 29, 2011
    JOURNAL FREE ACCESS
    To reduce the cost and time required to routinely perform the genetically modified organism (GMO) test, we developed a duplex quantitative real-time PCR method for a screening analysis simultaneously targeting an event-specific segment for GA21 and Cauliflower Mosaic Virus 35S promoter (P35S) segment [Oguchi et al., J. Food Hyg. Soc. Japan, 50, 117-125 (2009)]. To confirm the validity of the method, an interlaboratory collaborative study was conducted. In the collaborative study, conversion factors (Cfs), which are required to calculate the GMO amount (%), were first determined for two real-time PCR instruments, the ABI PRISM 7900HT and the ABI PRISM 7500. A blind test was then conducted. The limit of quantitation for both GA21 and P35S was estimated to be 0.5% or less. The trueness and precision were evaluated as the bias and reproducibility of the relative standard deviation (RSDR). The determined bias and RSDR were each less than 25%. We believe the developed method would be useful for the practical screening analysis of GM maize.
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