Estimation of Irradiation Doses of Raw Beef Liver Samples using 5,6-Dihydrothymidine as an Irradiation Marker.

The quantities of (5)- and (5)-5,6-dihydrothymidine (total DHdThd) in frozen beef liver samples were compared between those irradiated by an electron beam (EB) and those subjected to γ-irradiation. DNA extracted from the samples was enzymatically digested to nucleosides and analyzed by liquid chromatography-tandem mass spectrometry for total DHdThd and 2'-deoxythymidine (dThd). Total DHdThd was formed radiospecifically and dose-dependently and the dose-response curves of the ratio of total DHdThd to dThd (total DHdThd/dThd) were similar for both the EB- and γ-irradiated samples.

Enhancement of Pesticide Peak Response in GC-MS in the Presence of Multiple Co-Existing Reference Pesticides.

We carried out a collaborative study in six laboratories to confirm the universality of the enhancing effect of co-existing reference pesticides on the GC-MS peak response to a target pesticide (malathion, procymidone, or flucythrinate). First, we confirmed the response enhancement of the target pesticides with increasing numbers of co-existing reference pesticides in solution. Then, using diluted green soybean matrix, we analyzed the target pesticides with two types of matrix-matched calibration, containing the target pesticides or 166 other pesticides.

Rapid and Reliable Method for Determining Irradiation Histories of Ground Beef and Prawns by Measuring 5,6-Dihydrothymidine.

A rapid and reliable method for determining irradiation histories of ground beef and prawns was developed on the basis of a method for determining the irradiation history of beef liver by liquid chromatography-tandem mass spectrometry (LC-MS/MS) of 5,6-dihydrothymidine (DHdThd). Improvements in the method included the following: (1) 50% ethanol precipitation in the DNA extraction step was conducted before the RNase step, (2) snake venom phosphodiesterase I was used for DNA digestion to boost liberation of DHdThd, and (3) a matrix-matched calibration curve was used for determining DHdThd by LC-MS/MS analysis. This method successfully determined irradiation histories of ground beef and prawns.

[Trial for estimating the concentration of pesticide residues in the ingredients of processed foods].

If pesticide residues are detected at over the uniform limit (0.01 ppm) in processed foods, the maximum residue limits of pesticides in each ingredient should be considered. For that purpose, analysis of pesticide residues in the ingredients would be required, but in many cases it is difficult to obtain ingredients from the same lot, or the processed foods may have been manufactured overseas.

[Validation study on a rapid multi-residue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS].

A validation study was conducted on a rapid multiresidue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS. Pesticide residues in the vegetables or fruits were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride in the presence of citrate salts for buffering. The extract was purified with a double-layered cartridge column (graphite carbon black/primary secondary amine silica gel; GCB/PSA).

A simple and selective detection method for aristolochic acid in crude drugs using solid-phase extraction.

The official Japanese method for analyzing aristolochic acid I (AA-I) in Asiasarum root using conventional high-performance liquid chromatography (HPLC) is described in the Japanese Pharmacopoeia, Sixteenth Edition. Interfering peaks of AA-I sometimes appear after HPLC analysis of crude drugs. A selective analytical method is needed to determine definitively whether AA-I is present in crude drugs.

[Simultaneous determination of polyether antibiotics and macrolide anthelmintics in livestock products by liquid chromatography/tandem mass spectrometry].

A method using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of polyether antibiotics and macrolide anthelmintics in livestock products. The polyether antibiotics and macrolide anthelmintics were extracted from livestock products with acetonitrile and cleaned up with dispersive solid-phase extractions and a silica gel column. The quantification limits of polyether antibiotics and macrolide anthelmintics were 0.

[Determination of histamine in fish and fish products by tandem solid-phase extraction].

A simple and practical method was developed for the determination of histamine in fish and fish products by solid-phase extraction and fluorescence derivatization. Histamine was extracted with trichloroacetic acid. The extract was neutralized and diluted with phosphate buffer (pH 6.

[Preparation of samples for proficiency testing of pesticide residue analysis in processed foods].

To conduct proficiency testing for the analysis of pesticide residues in processed foods, fortified samples of retort curry and pancake were examined. In the case of retort curry, heating and mixing were necessary at the time of preparation to provide a homogenous analytical sample. A mixture of 4 carbamates and 11 organophosphorus pesticides was spiked and 14 of them showed consistent results in the samples.

[Basic study for the measurement of the bone mineral density of the calcaneus by using the radiographic contrast].

We performed a fundamental study for the measurement of the bone mineral density (BMD) of the calcaneus by using the radiographic contrast (RC). The RC of the bone radiography is proportional to the product of the thickness of the bone H(b), the gradient of the image detector system and the difference of the linear attenuation coefficient between the bone and the soft tissue. Therefore, the radiographic contrast per unit bone thickness (RC/H(b)) can be used as a good measure of the BMD.

[Rapid analysis of toxic heavy metals in foods for emergency response to health crisis].

A simple and rapid method for determination of intentional contamination with heavy metals in foods using inductively coupled plasma-atomic emission spectroscopy (ICP-AES) has been developed. The heavy metals were extracted with sulfuric acid in a disposable tube using a homogenizer. The extract was diluted with 1% HNO(3) solution and analyzed with ICP-AES.

[Multiresidue method for determination of pesticide residues in processed foods by GC/MS/MS].

A rapid and simple multiresidue method has been established for determination of pesticide residues in processed foods by GC/MS/MS. The pesticides were extracted with ethyl acetate, and were cleaned up with a double-layered SPE cartridge column (graphite carbon black/PSA silica gel). Recovery tests of 258 pesticides from five kinds of processed foods (dumpling, curry, French fries, fried chicken, fried fish) were performed at two different fortification levels of 0.

[Multiresidue method for determination of pesticide residues in processed foods by GC/MS].

A rapid and simple multiresidue method has been established for determination of pesticide residues in processed foods by GC/MS. The pesticides were extracted with ethyl acetate in the presence of anhydrous MgSO(4) in a disposable tube, using a homogenizer. The extract was concentrated and reconstituted in hexane, followed by acetonitrile-hexane partition to remove lipids.

[Determination of melamine in Chinese-made processed food].

A method using liquid chromatograph coupled with tandem mass spectrometer (LC/MS/MS) was developed for the determination of melamine in processed food. After extraction with 50% acetonitrile and clean-up with PSA and SCX, the quantification limit of melamine in processed food was 0.5 microg/g.

[Determination of pesticides in Chinese dumplings using liquid chromatography-tandem mass spectrometry].

A rapid and easy multiresidue method for determination of pesticide residues in Chinese dumplings using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed. Pesticide residues were extracted with ethyl acetate in the presence of anhydrous magnesium sulfate in a disposable tube using a homogenizer. The extract was concentrated and reconstituted in hexane, followed by acetonitrile-hexane partition to remove lipids.

[Determination of sulfonamides in livestock products and seafoods by liquid chromatography/tandem mass spectrometry using glass bead homogenization].

A 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.

Detection of irradiated meat, fish and their products by measuring 2-alkylcyclobutanones levels after frozen storage.

2-Alkylcyclobutanones, such as 2-dodecylcyclobutanone and 2-tetradecylcyclobutanone, were analyzed to assess the irradiation history of irradiated meats or fish, and cooked foods with irradiated ingredients, which had been stored frozen for up to one year. The purpose of the study was to show that irradiated meats could be detected even after having been stored in the distribution system. 2-Alkylcyclobutanones showed a small decrease in irradiated raw meats that had been stored frozen for one year.

Simultaneous analysis of 17 organochlorine pesticides in natural medicines by GC/MS with negative chemical ionization.

Many methods for the determination of pesticide residues in food have been reported. Although natural medicines should be confirmed to be as safe as food, few methods for the determination of pesticide residues in natural medicines have been reported. In this study, 17 organochlorine pesticides were detected in natural medicines using GC/MS with negative chemical ionization (NCI).

Analysis of 2-alkylcyclobutanones with accelerated solvent extraction to detect irradiated meat and fish.

A new analytical procedure has been developed to analyze 2-alkylcyclobutanones to detect gamma-ray-irradiated fat-containing foodstuffs. Samples were extracted with an accelerated solvent extraction system via hot and pressurized ethyl acetate in cells. A large amount of fat in the extract was precipitated and removed with filtration by standing at -20 degrees C after the addition of acetonitrile.