An analytical method based on LC-MS/MS was developed for the determination of formetanate hydrochloride in agricultural products. Formetanate hydrochloride was confirmed to be stable in acetonitrile. It was therefore extracted from samples with acetonitrile, and the crude extracts were purified using a combination of ethylenediamine-N-propyl silylation silica gel and graphite carbon mini columns. Formetanate hydrochloride in the resulting sample solutions was quantified by LC-MS/MS utilizing an external solvent calibration curve. The average recovery (n=5) of formetanate hydrochloride spiked in 10 types of agricultural products (brown rice, soybean, spinach, cabbage, potato, apple, orange, lime, nectarine and green tea) at the maximum residue limits (MRLs) or at a uniform limit of 0.01 mg/kg was 92.3–103%, with a relative standard deviation of 1.3–5.4%. The limit of quantitation of the developed method was calculated to be 0.01 mg/kg.
We conducted a study to examine aroma leakage from orange juice packed in gable-top paper containers for chilled distribution. Limonene, an aromatic component of orange juice, was considered as an index compound of aroma leakage, and its seepage on the surface of the container and concentration in the orange juice were measured by GC-MS for 12 commercial samples. After 3 days of storage, limonene was detected on the surface of 8 orange juice containers, and the concentration of limonene in the orange juice was found to have decreased. Thus, limonene leaked through the container within a few days, and the extent of leakage differed between containers, presumably depending upon their barrier properties. In addition, limonene was detected in green tea and milk that was stored together with the unopened orange juice containers at 4℃. The transference of orange aroma into milk was significant, because the contamination of the milk was confirmed by subjective sensory evaluation. This study suggests the possibility of transfer of aroma compounds through paper containers to other beverages.
Adverse events associated with health food use appear to be quite common. Nevertheless, even though severe adverse events should be reported to the Japanese government via public health centers, the number of cases reported is relatively small. To clarify this discrepancy and to understand how consumers and physicians act when they or their patients develop adverse events due to health food use, we conducted an internet questionnaire with consumers (preliminary survey: n=44,649; full survey: n=3,000), physicians (n=500), and pharmacists (n=500). During 2016, 17% of consumers who used health foods developed adverse events. However, only 11% of them reported their adverse events to public health centers. Most physicians and pharmacists did not report these cases to public health centers because they were unable to establish a clear cause-and-effect relationship. It is important to encourage not only consumers, but also physicians and pharmacists to report adverse events to public health centers.
A rapid LC-MS method was developed for determination of acromelic acids A and B, which are toxic constituents of Paralepistopsis acromelalga (=Clitocybe acromelalga), in mushroom samples. Acromelic acids were extracted twice with 50% methanol and the extract was passed through a syringe filter, and then analyzed by LC-MS. The LC separation was performed on a multi-mode ODS column. The recoveries of acromelic acids A and B spiked into blank mushroom samples at 2.5 μg/g were 93 and 74%, respectively. This method was applied to the remaining mushroom sample from a food poisoning case. Acromelic acids A and B were detected at 2.0 and 1.4 μg/g, respectively, in the remaining sample. Another toxic constituent, which appeared to be clitidine, was also detected in the sample.