Estimation of daily intake of food additives by Japanese young children using the market basket method in 2018.

To estimate the daily intake of food additives by young children aged 1-6 years in Japan, an intake survey was conducted in 2018 using the market basket method for food additives, including twelve types of colourants, three kinds of preservatives, three kinds of sweeteners and two kinds of food manufacturing agents. A list of the daily consumption of processed foods was prepared based on a special survey (MHLW 2011) and used for the estimation. The results of the survey showed that the food additives with the highest daily intake were phosphorus compounds (phosphoric acid and its salts; 11.2 mg/kg bw/day, expressed as phosphorus), followed by propylene glycol (0.80 mg/kg bw/day). The daily intake of other food additives ranged from 0 to 0.20 mg/kg bw/day. The estimated daily intake of each food additives by young children was compared with the acceptable daily intake (ADI) or maximum tolerable daily intake (MTDI). The highest ratio of the estimated daily intake to ADI was 3.2% for propylene glycol, whereas the ratios of the estimated daily intake to ADI for colourants, preservatives and sweeteners ranged from 0 to 1.1% (benzoic acid). The ratio of the estimated daily intake to MTDI for phosphorus compounds was 16%.

[Validation of Method for Nitrite Determination in Foods].

In general, nitrite in food is extracted under slightly alkaline conditions, deproteinized, and analyzed by a colorimetric method using color development by diazotization. However, depending on the sample, the sample solution may become cloudy and difficult to filter by the deproteinization treatment of the analytical method. Recently, an improved analytical method that solves these problems has been reported. Therefore, a validation study was performed on the improved analytical method was performed. The concentrations of sodium nitrite added to cod roe, fish sausage, and ham, which were not labeled with sodium nitrite, were set at the upper limits of the standards for use. We set the target values of 70-120% for trueness, less than 15% for intralaboratory reproducibility, and less than intralaboratory reproducibility for repeatability. As a result, the target values were met for the three samples verified: 88-92% for trueness, 2.0-3.0% for repeatability, and 3.2-4.3% for intralaboratory reproducibility. In addition, an interlaboratory study was conducted by eight institutes on the improved analytical method for nitrite. At each institution, sodium nitrite was added to the same three samples as in the validation study, at concentrations equivalent to twice the lower limit of quantification and the upper limit of the standards for use and analyzed in triplicate. The estimated trueness from the obtained analyses ranged from 82 to 95%, the repeatability ranged from 2.3 to 5.8%, and the inter-room reproducibility ranged from 3.5 to 11%. Thus, the improved analytical method could be useful for determining nitrite in foods.

Subchronic toxicity evaluation of isoeugenyl methyl ether in F344/DuCrj rats by 13-week oral administration.

Isoeugenyl methyl ether (CAS No. 93-16-3) is a food additive used as a nature identical flavoring agent. To determine the toxicity profile and the no-observed-adverse-effect level (NOAEL), we performed a subchronic toxicity test in male and female F344/DuCrj rats by intragastric administration of isoeugenyl methyl ether at doses of 8, 40, and 200 mg/kg body weight (BW)/day for 13 weeks. In this study, BW gain in the male 200 mg/kg BW/day group was decreased from week 9. In serum biochemistry, decreased triglycerides were observed in the male 200 mg/kg BW/day group. In organ weights, increases in both absolute and relative liver weights were observed in both sexes in the 200 mg/kg BW/day group. In histopathological examination, hepatocyte hypertrophy was observed in the male 200 mg/kg BW/day group. Based on these results, we concluded that the main target organ of isoeugenyl methyl ether was the liver and that the NOAEL of isoeugenyl methyl ether for both male and female F344/DuCrj rats was estimated to be 40 mg/kg BW/day.

Determination of starting materials, intermediates, and subsidiary colors in the color additive Food Red No. 106 (Sulforhodamine B) using high-performance liquid chromatography.

The main subsidiary color of structure in Food Red No. 106 (R106) was identified to be a desethyl derivative (R106-SubA). High-performance liquid chromatography (HPLC) was performed for the quantitative determination of benzaldehyde-2,4-disulfonic acid, N,N-diethyl-m-aminophenol, leuco acid, pyrone acid, R106-SubA, etc. in R106. An ammonium acetate solution (20mM) and acetonitrile:water (7:3) were used to stabilize the retention time of the HPLC analytes. The linearity of the calibration curves was in the range of 0.05-10µg/mL, with good correlation coefficients (R2>0.9983). The recoveries of impurities at levels 0.1%, 0.5% and 1% ranged from 94.2% to 106.6% with relative standard deviations of 0.1%-1.0%. While surveying commercial R106, the amounts obtained by area% determination were similar to those obtained by the calibration-curve determination. The area% determination by HPLC for the determinations of impurities in R106 is a simple and reliable method and can be applied in routine analysis.

Solubility Testing of Sucrose Esters of Fatty Acids in International Food Additive Specifications.

We investigated the solubility of 10 samples of sucrose esters of fatty acids (SEFA) products that are commercially available worldwide as food additives (emulsifiers). Although one sample dissolved transparently in both water and ethanol, other samples produced white turbidity and/or precipitates and did not meet the solubility criterion established by the Joint Food and Agriculture Organization of the United Nations (FAO)/WHO Expert Committee on Food Additives (JECFA). When the sample solutions were heated, the solubility in both water and ethanol increased. All of the samples dissolved transparently in ethanol, and dispersed and became white without producing precipitates in water. The present study suggests that the current solubility criterion of the JECFA SEFA specifications needs to be revised.

An IC-MS/MS Method for the Determination of 1-Hydroxyethylidene-1,1-diphosphonic Acid on Uncooked Foods Treated with Peracetic Acid-Based Sanitizers.

A rapid, sensitive, and specific analytical method for the determination of 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP) on uncooked foods after treatment with a peracetic acid-based sanitizer (PAS) was developed. The method involves simple sample preparation steps and analysis using ion chromatography (IC) coupled with tandem mass spectrometry (MS/MS). The quantification limits of HEDP on uncooked foods are 0.007 mg/kg for vegetables and fruits and 0.2 mg/kg for meats. The recovery and relative standard deviation (RSD) of HEDP analyses of uncooked foods ranged from 73.9 to 103.8% and 1.9 to 12.6%, respectively. The method's accuracy and precision were evaluated by inter-day recovery tests. The recovery for all samples ranged from 93.6 to 101.2%, and the within-laboratory repeatability and reproducibility were evaluated based on RSD values, which were less than 6.9 and 11.5%, respectively. Analyses of PAS-treated fruits and vegetables using the developed method indicated levels of HEDP ranging from 0.008 to 0.351 mg/kg. Therefore, the results of the present study suggest that the proposed method is an accurate, precise, and reliable way to determine residual HEDP levels on PAS-treated uncooked foods.

Development of an HPLC Method with an ODS Column to Determine Low Levels of Aspartame Diastereomers in Aspartame.

α-L-Aspartyl-D-phenylalanine methyl ester (L, D-APM) and α-D-aspartyl-L-phenylalanine methyl ester (D, L-APM) are diastereomers of aspartame (N-L-α-Aspartyl-L-phenylalanine-1-methyl ester, L, L-APM). The Joint FAO/WHO Expert Committee on Food Additives has set 0.04 wt% as the maximum permitted level of the sum of L, D-APM and D, L-APM in commercially available L, L-APM. In this study, we developed and validated a simple high-performance liquid chromatography (HPLC) method using an ODS column to determine L, D-APM and D, L-APM in L, L-APM. The limits of detection and quantification, respectively, of L, D-APM and D, L-APM were found to be 0.0012 wt% and 0.004 wt%. This method gave excellent accuracy, repeatability, and reproducibility in a recovery test performed on five different days. Moreover, the method was successfully applied to the determination of these diastereomers in commercial L, L-APM samples. Thus, the developed method is a simple, useful, and practical tool for determining L, D-APM and D, L-APM levels in L, L-APM.

A simple and rapid chromatographic method to determine unauthorized basic colorants (rhodamine B, auramine O, and pararosaniline) in processed foods.

A simple and rapid high-performance liquid chromatography (HPLC) method to determine basic colorants such as pararosaniline (PA), auramine O (AO), and rhodamine B (RB) in various processed foods was developed. Linearity of the calibration curves ranged from 0.05 to 50 µg/mL for PA and 0.05-100 µg/mL for AO and RB. The detection and quantification limits (LOD and LOQ) of the basic colorants, which were evaluated as signal-to-noise ratios of 3 for LOD and 10 for LOQ, ranged from 0.0125 to 0.05 and 0.025 to 0.125 µg/g, respectively. The recoveries and relative standard deviations of three basic colorants in six processed foods, namely, chili sauce, curry paste, gochujang (hot pepper paste), tandoori chicken (roasted chicken prepared with yogurt and spices), powder soup, and shrimp powder ranged from 70.2% to 102.8% and 0.8% to 8.0%, respectively. The intraday precision of the recovery test ranged from 1.7% to 4.5%, whereas the interday precision ranged from 3.7% to 7.7%. The reported method has been successfully applied to basic colorant determination in various processed foods such as fat-based food matrices (curry paste and tandoori chicken), chili products (gochujang and chili sauce), and protein-based products (shrimp powder and powder soup). Thin layer chromatography and liquid chromatography/mass spectrometry methods for the determination of basic colorants in processed foods were also developed for rapid analysis and identification, respectively. These methods are very useful for monitoring unauthorized basic colorants in inspection centers or quarantine laboratories in many countries.

[Test method of methanol content in detergent].

A test method of methanol content in detergent using a headspace-GC method was established. A 1 g aliquot of test sample was mixed with 0.4 mg of 2-propanol and made up to 20 mL with water. Then, 5 mL of test solution was placed in a headspace vial. The vial was sealed and incubated for 30 min at 60°C, then the headspace gas was analyzed by GC-FID. The recovery from spiked 1 mg/g of methanol was 95.6-100.6%. The determination limit was 0.1 mg/g. Using this method, the methanol content in 14 kinds of detergents was quantified. Methanol was detected from two detergents at the levels of 0.13 and 0.27 mg/g.