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Volume 49 (2008)
- Issue 6 Pages 381-
- Issue 5 Pages 333-
- Issue 4 Pages 261-
- Issue 3 Pages 125-
- Issue 2 Pages 63-
- Issue 1 Pages 1-
Volume 49, Issue 6
Displaying 1-8 of 8 articles from this issue
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Originals
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Hiroko KAJITA, Eriko HATAKEYAMA2008 Volume 49 Issue 6 Pages 381-389
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSA rapid multiresidue method was developed for determination of 98 veterinary drugs in livestock products and fish by LC/MS/MS. The drugs were extracted with methanol, and the extracted solution was diluted with water. The methanol concentration was adjusted to 50%, and finally the diluted solution was filtered through a microfiltration membrane (0.02 μm diameter pore size) prior to LC/MS/MS. Recoveries of 87 drugs from 4 foods (milk, egg, rainbow trout and cattle muscle) fortified at 0.2 μg/g were in the range of 50-150% with a coefficient of variation (%) of less than 20%. The values obtained by this method from livestock products containing antibiotics were similar to those obtained by the official methods. This proposed method is expected to be useful as a multiresidue analysis method for screening of veterinary drugs in livestock products and fish.View full abstractDownload PDF (615K) -
Eiji UENO, Yuka KABASHIMA, Harumi OSHIMA, Tsutomu OHNO2008 Volume 49 Issue 6 Pages 390-398
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSA sensitive and quantitative multiresidue method using NCI mode GC/MS and GC-micro ECD for determining pesticides in animal and fishery products was established. The crude sample extract obtained by acetone-hexane extraction for solid samples or acetonitrile extraction for liquid samples was cleaned up with a GPC/SPE system. The first GPC pesticide fraction containing lipids and pigments was selectively collected, and loaded directly onto a graphitized carbon/PSA 2-layered column. After the second GPC pesticide fraction was collected, the 2-layered column was eluted with acetone-hexane (3 : 7). The combined eluate was subjected to NCI-SIM/Scan mode GC/MS for semi-quantification. After fractionation by Florisil cartridge column SPE, each fraction was subjected to dual-column GC-micro ECD for quantification. Average recoveries (n=5) of pesticides, except for chlorothalonil and some others, from fortified samples ranged from 76.8% to 107.9% with RSD values of <9.7%.View full abstractDownload PDF (975K)
Notes
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Naoki MOCHIZUKI, Eri AOKI, Keiko SUGA, Rie ISHII, Masakazu HORIE2008 Volume 49 Issue 6 Pages 399-402
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSA quantitative analysis method using LC/MS/MS of chloramphenicol (CAP) in propolis extract (ethanol extract) has been established. Extraction of CAP from propolis extract was performed by adding water, followed by salting-out with sodium chloride. Through this procedure, the wax components of propolis extract could be effectively removed. LC separation was performed with a reverse-phase column (Mightysil RP-18 GP Aqua, 2.0 mm×150 mm, 5 μm), using 10 mmol/L of ammonium acetate-acetonitrile (75 : 25) as a mobile phase. The flow rate was 0.2 mL/min. Ionization was performed by electrospray ionization (ESI) in the negative mode. The detection and quantification limits of CAP in propolis extract were 0.05 and 0.15 ng/g, respectively, and the recovery rate (spiked CAP level was 0.5 ng/g) was 111.2%. When eight samples of propolis extract products on the market were analyzed using this method, CAP was not detected (N.D.) in any of the samples.View full abstractDownload PDF (414K) -
Kunihiko TAKAHASHI, Masakazu HORIE, Yoshihumi HIROSE2008 Volume 49 Issue 6 Pages 403-406
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSA simple determination method of diphenyl (DP) and o-phenylphenol (OPP) in agricultural products by GC/MS was examined. DP and OPP were extracted with ethyl acetate in the presence of anh. sodium sulfate. After addition of n-butanol, the extract solution was concentrated. Clean-up was achieved by shaking with graphitized bulk carbon (Supelclean ENVI-Carb). Addition of polyethylene glycol sharpened the OPP peak on GC/MS analysis.
The recoveries from 9 kinds of agricultural products spiked at 0.01 and 0.5 μg/g each were mostly in the range of 70 to 120%, except for 50% recovery of OPP from barley spiked at 0.01 μg/g. The quantification limits (S/N ≥10) of DP and OPP were 0.0013 and 0.005 μg/g (0.0025 and 0.01 μg/g in barley and soybean), respectively.View full abstractDownload PDF (389K) -
Tetsuya AKIBA, Tatsuya TANAKA, Teruyoshi ARAI, Yukinao HAYASHI, Kohji ...2008 Volume 49 Issue 6 Pages 407-410
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSFactors such as low recovery rate and food contaminants may be responsible for the difficulty of detecting Norovirus (NV) by PCR in foodborne outbreaks. To detect NV more efficiently, we introduced a bacterial treatment, in which concentrated samples were incubated overnight with Klebsiella oxytoca at 35°C before RNA extraction using the standard protocol. Recovery rates of NVs (G I/8 or G II/13) added to food suspensions in the modified method were compared with those in the standard method by quantification of NV RNAs using real-time PCR. Recovery rates in the modified method were 8.6% for G I/8 and 11.6% for G II/13 in 18 oyster samples and 13.9% for G I/8 and 19.6% for G II/13 in 15 other food samples, while those in the standard method were 0.3% for G I/8 and 0.5% for G II/13 in the oyster samples and 1.9% for G I/8 and 7.9% for G II/13 in the other food samples. These results indicate that the bacterial treatment increase the recovery of NV from foods such as oysters, suggesting that the modified method will be useful for NV detection in food samples.View full abstractDownload PDF (442K) -
Mizuka FUJITA, Shuzo TAGUCHI, Hirotaka OBANA2008 Volume 49 Issue 6 Pages 411-415
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSA simple and rapid method using liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) was developed for the determination of 25 kinds of sulfonamides in livestock products and seafoods. The sulfonamides were extracted with acetonitrile by glass bead homogenization and cleaned up with a tandem-connected ODS and basic alumina column. The quantification limits of 25 kinds of sulfonamides were 0.0025-0.005 μg/g. When two sulfonamides of specific samples were excluded, the recoveries and relative standard deviations were 70 to 120% and less than 15%. These results show that the developed method, which minimizes the matrix effect, offers high precision and should be useful for the determination of sulfonamides in livestock products and seafoods.View full abstractDownload PDF (434K)
Reports
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Miho FUJITA, Wataru TAMURA, Takahiro TOZAWA, Takashi KOMETANI2008 Volume 49 Issue 6 Pages 416-421
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSTo ensure the safety of processed foods, we developed a method for simultaneous determination of residual veterinary drugs in some processed foods. Eighty-nine compounds were selected for the analysis based on reports of illegal use of the veterinary drugs and our research information. In our LC/MS/MS system, an Atlantis C18 column, which could separate a wide range of compounds, was used with a gradient system of 0.1% formic acid-acetonitrile containing 0.1% formic acid as the mobile phase. Sharp and symmetrical peaks with sufficient signal intensity were obtained. In this system, the recovery rates of detected veterinary drugs in processed foods were mostly in the range of 60-120%. Therefore, it is considered that this method is suitable for screening of residual veterinary drugs in processed foods.View full abstractDownload PDF (379K) -
Nobuyuki KADOTA, Hiroko NARITA, Ritsuko MURAKAMI, Tamao NOGUCHI2008 Volume 49 Issue 6 Pages 422-427
Published: December 01, 2008
Released on J-STAGE: January 21, 2009
JOURNAL FREE ACCESSToxicity study was conducted using an official method (mouse assay) on 77 individual starfishes of the Astropecten genus collected in 5 sites inside Toyama Bay during the period from July 2002 to January 2003. Three kinds of starfishes were toxic, i.e., Astropecten polyacanthus, A. scoparius, and A. latespinosus meissner. Of A. polyacanthus. Those collected in the winter and spring were highly toxic, and there were regional differences in toxicity. The toxicity of A. latespinosus meissner, which inhibits only Himi, was less than that of A. polyacanthus. The toxicity of A. scoparius was weak. Toxic components were extracted and analyzed by LC/MS. Tetrodotoxin and related substances were confirmed to be present in all 3 kinds of starfishes.View full abstractDownload PDF (512K)
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