[A Simple and Rapid Analysis Method for Nonvolatile Amines via LC-MS/MS].

In order to quickly analyze 8 types of nonvolatile amine, such as histamine, a simple analytical method was developed. A test solution was prepared only by diluting and filtering a trichloroacetic acid extract before analysis via LC-MS/MS.As a result of the additive recovery test with 11 types of food, including fresh seafood, seafood processed products, and other processed foods, all amines had an accuracy in the range of 70 to 120% with a repeatability of less than 15% RSD in 9 types of food. This confirmed the validity of the analytical method with the lower limit of quantification between 5 to 6 mg/kg.

[Evaluation of the Pesticide analysis in Agricultural Products Using the Self-Cleaning Ion Source GC-MS/MS].

We evaluated an analytical method to detect pesticide residues in agricultural products through the use of a self-cleaning ion source GC-MS/MS. The self-cleaning ion source minimizes ion source contamination by ensuring that hydrogen is pumped into the source at a fixed pressure after or during measurement. When we employed our self-cleaning ion source GC-MS/MS technique to analyze pesticides residues in agricultural products, we observed that pollution of the ion source surface was considerably reduced. Good peak sensitivity was obtained for 251 pesticides, and a calibration curve with a coefficient of determination (R2) of 0.990 or higher was obtained for 253 pesticides. In the recovery test with 6 types of agricultural products, the acceptability criteria of recovery (70-120%) and standard deviation of repeatability (RSD<25%) was met in 180-221 pesticides.

[Pesticide Analysis in Agricultural Products by GC-MS/MS Using STQ Method].

As a method to detect pesticide residues in agricultural products, we evaluated the pretreatment of agricultural product samples by the solid-phase extracton technique with QuEChERS (STQ) method followed by GC-MS/MS with large-volume injection using a stomach-type glass-lined injector. This method satisfied the target criteria of recovery (70-120%) and the standard deviation of repeatability (RSD<25%) in 238-282 pesticides found in six types of agricultural products.

[Evaluation of an Analytical Method Using GC-MS/MS and a 3-Layer Solid Phase Extraction Mini-Column for Pesticide Residues in Agricultural Products].

We developed a simple rapid analysis of multi-pesticide residues in agricultural products. In this study, we attempted to simplify the purification process, and reduce the amount and type of solvent used. The test solution was prepared by clean-up, a 0.5 mL aliquot of QuEChERS extract solution of agricultural products using a 3-layer solid-phase (C18/SAX/PSA) extraction mini-column, and the test solution was subjected to GC-MS/MS analysis, modified with a large volume injection and a stomach-type glass-lined injector. This method met the acceptability criteria of recovery (70-120%) and standard deviation of repeatability (RSD<25%) in 241-331 pesticides in 8 types of agricultural products.

[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. In both cases, the response-enhancing effect of co-existing pesticides was confirmed in all laboratories. The enhancement was reduced by addition of green soybean matrix to the sample and calibration solutions. Our results show that it is necessary to estimate the peak response-enhancing effect of co-existing pesticides in the calibration solution to obtain accurate results with GC-MS determination. The enhancing effect could be reduced by addition of food matrix to the sample and calibration solutions.