Are we using more sugar substitutes? Wastewater analysis reveals differences and rising trends in artificial sweetener usage in Swedish urban catchments.

The market for artificial sweeteners as substitutes for conventional sugar (sucrose) is growing, despite potential health risks associated with their intake. Estimating population usage of artificial sweeteners is therefore crucial, and wastewater analysis can serve as a complement to existing methods. This study evaluated spatial and temporal usage of artificial sweeteners in five Swedish communities based on wastewater analysis. We further compared their levels measured in wastewater with the restrictions during the COVID-19 pandemic in Sweden and assessed health risks to the Swedish population. Influent wastewater samples (n = 194) collected in March 2019-February 2022 from communities in central and southern Sweden were analyzed for acesulfame, saccharin, and sucralose using liquid-chromatography coupled with tandem mass spectrometry. Spatial differences in loads for individual artificial sweetener were observed, with sucralose being higher in Kalmar (southern Sweden), and acesulfame and saccharin in Enköping and Östhammar (central Sweden). Based on sucrose equivalent doses, all communities showed a consistent prevalence pattern of sucralose > acesulfame > saccharin. Four communities with relatively short monitoring periods showed no apparent temporal changes in usage, but the four-year monitoring in Uppsala revealed a significant (p < 0.05) annual increase of ∼19 % for sucralose, ∼9 % for acesulfame and ∼8 % for saccharin. This trend showed no instant or delayed effects from COVID-19 restrictions, reflecting positively on the studied population which retained similar exposure to the artificial sweeteners despite potential pandemic stresses. Among the three artificial sweeteners, only acesulfame's levels were at the lower end of the health-related threshold for consumption of artificially sweetened beverages; yet, all were far below the acceptable daily intake, indicating no appreciable health risks. Our study provided valuable, pilot insights into the spatio-temporal usage of artificial sweeteners in Sweden and their associated health risks. This shows the usefulness of wastewater analysis for public health authorities wishing to assess future relevant interventions.

Acesulfame and other artificial sweeteners in a wastewater treatment plant in Alberta, Canada: Occurrence, degradation, and emission.

Acesulfame (ACE), sucralose (SUC), cyclamate (CYC), and saccharin (SAC) are widely used artificial sweeteners that undergo negligible metabolism in the human body, and thus ubiquitously exist in wastewater treatment plants (WWTPs). Due to their persistence in WWTPs, ACE and SUC are found in natural waters globally. Wastewater samples were collected from the primary influent, primary effluent, secondary effluent, and final effluent of a WWTP in Alberta, Canada between August 2022 and February 2023, and the artificial sweeteners concentrations were measured by LC-MS/MS. Using wastewater-based epidemiology, the daily per capita consumption of ACE in the studied wastewater treatment plant catchment was estimated to be the highest in the world. Similar to other studies, the removal efficiency in WWTP was high for SAC and CYC, but low or even negative for SUC. However, ACE removal remained surprisingly high (>96%), even in the cold Canadian winter months. This result may indicate a further adaptation of microorganisms capable of biodegrading ACE in WWTP. The estimated per capita discharge into the environment of ACE, CYC, and SAC is low in Alberta due to the prevalent utilization of secondary treatment throughout the province, but is 17.4-18.8 times higher in Canada, since only 70.3% of total discharged wastewater in Canada undergoes secondary treatment.

Untreated wastewater impact and environmental risk assessment of artificial sweeteners in river water and sediments of the Danube River Basin in Serbia.

Artificial sweeteners are receiving increasing attention as newly recognized emerging contaminants that mainly reach the aquatic environment through the discharge of municipal wastewater containing large amount of these compounds. In this study, the impact of raw untreated wastewater discharges on the levels and the water/sediment distribution of artificial sweeteners in the Danube River and its largest tributaries in Serbia was evaluated, and a comprehensive assessment of environmental risks for freshwater and benthic organisms was performed. Acesulfame and sucralose were detected in all river water samples (100%), while saccharin (59%) and cyclamate (12%) were less frequently found, indicating long-term continuous sewage-derived pollution. Aspartame (100%) and neotame (60%) were the only artificial sweeteners recorded in the sediment samples due to their preference to sorb to particulate matter in the water/sediment system. In terms of ecotoxicological risk, a low risk for aquatic organisms was determined at the detected levels of saccharin in river water, while a high to medium risk was found for benthic biota at the concentrations of neotame and aspartame detected in sediments. The largest contribution to the pollution of the Danube River Basin with artificial sweeteners, and consequently the highest environmental risk, was determined in the two largest cities, the capital Belgrade and Novi Sad, which raises the issue of transboundary pollution.

Levels, consumption, and variations of eight artificial sweeteners in the wastewater treatment plants of Dalian city, China.

Artificial sweeteners (ASs) are emerging contaminants in the environment, primarily derived from wastewater treatment plant (WWTP) effluents. In this study, the influents and effluents of three WWTPs in the Dalian urban area, China, were analyzed for the distribution of 8 typical ASs to investigate their seasonal fluctuations in the WWTPs. The results showed that acesulfame (ACE), sucralose (SUC), cyclamate (CYC), and saccharin (SAC) were both detected in the influent and effluent water samples of WWTPs, with concentrations ranging from not detected (ND) to 14.02 µg·L-1. In addition, SUC was the most abundant ASs type, accounting for 40 %-49 % and 78 %-96 % of the total ASs in the influent and effluent water, respectively. The WWTPs revealed high removal efficiencies of CYC, SAC, and ACE, while the SUC removal efficiency was poor (26 % ± 36 %). The ACE and SUC concentrations were higher in spring and summer, and all ASs showed lower levels in winter, which may be caused by the high consumption of ice-cream in warmer months. The per capita ASs loads in the WWTPs were determined in this study based on the wastewater analysis results. The calculated per capita daily mas loads for individual ASs ranged from 0.45 g·d-1·1000p-1 (ACE) to 2.04 g·d-1·1000p-1 (SUC). In addition, the relationship between per capita ASs consumption and socioeconomic status showed no significant correlation.

Non-Nutritive Sweeteners in Human Amniotic Fluid and Cord Blood: Evidence of Transplacental Fetal Exposure.

OBJECTIVE: This study aimed to investigate human fetal exposure to non-nutritive sweeteners (NNS) by analyzing amniotic fluid and umbilical cord blood. STUDY DESIGN: Concentrations of four NNS (acesulfame-potassium [ace-K], saccharin, steviol glucuronide, and sucralose) were measured in amniotic fluid (n = 13) and cord blood samples (n = 15) using liquid chromatography-mass spectrometry. Amniotic fluid samples were obtained for research purposes at the time of term elective cesarean birth or clinically indicated third trimester amnioreduction at Mercy Hospital for Women (Melbourne, Australia). All except four women were in the fasting state. Cord blood samples were obtained from an independent cohort of newborns whose mothers were enrolled in a separate clinical trial at the National Institutes of Health. RESULTS: Ten of 13 amniotic fluid samples contained at least one NNS (ace-K, saccharin, steviol glucuronide, and/or sucralose). Maximum amniotic fluid NNS concentrations of ace-K, saccharin, steviol glucuronide, and sucralose were 78.9, 55.9, 93.5, and 30.6 ng/mL, respectively. Ace-K and saccharin were present in 100% and 80% of the cord blood samples, with maximal concentrations of 6.5 and 2.7 ng/mL, respectively. Sucralose was not detected and steviol glucuronide was not measurable in any of the cord blood samples. CONCLUSION: Our results provide evidence of human transplacental transmission of NNS. Based on results predominantly obtained from rodent models, we speculate that NNS exposure may adversely influence the offsprings' metabolic health. Well-designed, prospective clinical trials are necessary to understand the impact of NNS intake during pregnancy on human development and long-term health. KEY POINTS: · NNS consumption during pregnancy has increased in recent years.. · Maternal NNS intake during pregnancy is associated with preterm birth and higher infant weight gain in epidemiologic studies.. · In rodents, in utero NNS exposure induces metabolic abnormalities in mothers and their offspring, alters offspring gut microbiota composition, and promotes sweet taste preference in adulthood.. · It is presently unknown whether and to what degree maternal NNS ingestion in humans leads to direct in utero exposure.. · This study provides the first evidence of in utero NNS exposure in humans and highlights the urgent need to investigate clinical consequences of early life NNS exposure on metabolism, weight, taste preference, and general health..

Suspect screening of pharmaceuticals, illicit drugs, pesticides, and other emerging contaminants in Argentinean Piaractus mesopotamicus, a fish species used for local consumption and export.

The widespread distribution of contaminants of emerging concern (CECs) is a major concern due to their potential effects on human health and the environment. The insufficient sewage treatment plant infrastructures is a global problem most accentuated in less developed countries and results in the discharge of CECs to water bodies. Pacu (Piaractus mesopotamicus) is a ray-finned freshwater fish species native to the Paraná basin. It is also the most produced aquaculture fish species in Argentina since 2012. Though uninvestigated to date, the occurrence of CECs in pacu may be of high relevance due to production volumes and relevance to human exposure through fish consumption. In this study, we applied a high-resolution mass spectrometry screening method to qualitatively analyze over 100 CECs in pacu. Four extraction/cleanup methods were tested on pooled pacu fillet, including solid-phase extraction and QuEChERS. The method that produced the highest number of detections was selected for further analysis of pacu purchased in supermarkets and fish markets in Argentina between 2017 and 2020. Residues of pesticides, antibiotics, pharmaceuticals, personal care products, plasticizers, sweeteners, drug metabolites, stimulants, and illegal drugs were detected in the samples. A total of 38 CECs were detected, ranging between 24 and 35 CECs per individual sample. 100% of the samples had positive detections of caffeine, 1,7-dimethylxanthine, xanthine, benzoylecgonine, methylparaben, ethylparaben, bis(2-ethylhexyl) phthalate (DEHP), metolachlor, carbendazim, salicylic acid, 2,4-D, saccharin, cyclamate, and dodecanedioic acid. Mappings generated with correspondence analysis were used to explore similarities/dissimilarities among the detected compounds. To our knowledge this is the first report of saccharin, cyclamate, 2,4 - D, carbendazim, metolachlor, ethylparaben, propylparben, bisphenol A, DEHP, and benzotriazole in fish from Argentina, and the first report on the presence of lisinopril, metropolol acid and dodecanedioic acid in fish worldwide.

Young population consume twice as much artificial sweetener than the general population - A wastewater-based assessment in China.

Understanding artificial sweetener consumption patterns and levels in different demographics is important for formulating public health policies on controlling sugar consumption. There is a considerable knowledge gap with respect to the pattern of artificial sweetener consumption in China. To narrow this gap, wastewater analysis was used to assess the temporal patterns of consumption of seven artificial sweeteners in an urban population and a university town in a megacity in South China over a one-year period. Daily influent wastewater samples were collected from an urban catchment and weekly samples collected from a university sub-catchment. Population normalized per capita consumption of the four detected artificial sweeteners (cyclamate, acesulfame, sucralose and saccharin) in the university catchment (1.0-5.9 mg d-1 p-1) was much higher than those in urban catchment (0.5-1.3 mg d-1 p-1), indicating younger population consume more artificial sweeteners than the general population. The daily consumption of artificial sweeteners was found to be stable throughout the week in the urban catchment. Time-series analysis showed that an average increase in temperature of 1 °C was associated with an increase consumption of 33 µg d-1 p-1 for acesulfame, 15 µg d-1 p-1 for sucralose and 14 µg d-1 p-1 for saccharin. This was the first study that objectively quantified the greater consumption of artificial sweeteners (proxy for consumption of artificially sweetened food and beverages) in a younger age group when compared to the general population, which could potentially pose a risk of health related diseases.

The Effects of Nonnutritive Sweeteners on the Cariogenic Potential of Oral Microbiome.

Nonnutritive sweeteners (NNSs) are sugar substitutes widely used to reduce the negative health effects of excessive sugar consumption. Dental caries, one of the most prevalent chronic diseases globally, results from a pathogenic biofilm with microecological imbalance and frequent exposure to sugars. Some research has shown that certain NNSs possess less cariogenic potential than sucrose, indicating their putative effect on oral microbiome. To uncover the alterations of acidogenic pathogens and alkali-generating commensals, as well as the biofilm cariogenic potential under the influence of NNSs, we selected four common NNSs (acesulfame-K, aspartame, saccharin, and sucralose) and established single-, dual-, and multispecies in vitro culture model to assess their effects on Streptococcus mutans (S. mutans) and/or Streptococcus sanguinis (S. sanguinis) compared to sucrose with the same sweetness. The results showed that NNSs significantly suppressed the planktonic growth, acid production, and biofilm formation of S. mutans or S. sanguinis compared with sucrose in single-species cultures. Additionally, decreased S. mutans/S. sanguinis ratio, less EPS generation, and higher pH value were observed in dual-species and saliva-derived multispecies biofilms with supplementary NNSs. Collectively, this study demonstrates that NNSs inhibit the cariogenic potential of biofilms by maintaining microbial equilibrium, thus having a promising prospect as anticaries agents.

Fullerenol as a water-soluble MALDI-MS matrix for rapid analysis of small molecules and efficient quantification of saccharin sodium in foods.

Due to the strong background interferences in the low-mass region and poor reproducibility of conventional organic matrices, it is of great importance to develop a novel matrix for matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) to qualitatively and quantitatively analyze small molecules. In this work, water-soluble fullerenol C60(OH)24-26 was selected as a MALDI matrix for the analysis of low-molecular-weight compounds in consideration of optical absorption property, water solubility and stability. Compared with the traditional matrices, fullerenol demonstrated lower background interference and stronger peak intensity. In addition, the hydrophilic fullerenol could avoid the heterogeneous crystallization in sample preparation, increase the reproducibility and sensitivity of MALDI-MS, and ameliorate quantitative analysis of small molecules. With saccharin as model analyte, quantitative analysis was carried out using fullerenol as matrix. The results demonstrated satisfying reproducibility and good tolerance to salt. The limit-of-detection of the quantitative analysis was as low as 4 pmol, and the linear range is 1-100 µg mL-1 with R2 greater than 0.99. The analytical results also showed excellent precision and accuracy, low matrix effect and good recovery rate. Fullerenol as a potential matrix was further validated in the quantification of saccharin sodium in different real food samples, such as nuts and drinks. This work not only confirms the potential of fullerenol for the quantitative analysis in food field, but also provides a new technique for rapid analysis of small molecules.

Efficient sensing of saccharin through interference synthesis of gum ghatti capped silver nanoparticles.

The presence of saccharin (SH) could be efficiently sensed (in the concentration range of 5 × 10-5 M to 5 × 10-1 M) through the interference synthesis of gum ghatti (GG) capped silver nanoparticles (GGAgNps). The synthesis used sodium borohydride and gum ghatti (GG) as the reducing and capping agents respectively. The strong hydrogen-bonding recognition between GG and SH was responsible for the interference. The intensity of the SPR peak of GGAgNps was found linearly dependent on [SH]. The SH detection was further enhanced when combo capping comprising of GG and chitosan (Ch) (in 1:1 weight ratio) was used while the use of gum acacia (GA) in place of Ch (in combo) decreased the detection sensitivity. The combo polysaccharide solutions had non-Newtonian behaviour and shear thinning property like GG. The method was also applied for the successful detection of SH in commercially available real juice samples.

Measurement of Saccharin and trans-Resveratrol Metabolites in Urine as Adherence Markers for Small Quantity Lipid-Based Nutrient Supplement Consumption.

Saccharin and trans-resveratrol were incorporated into small quantity lipid-based nutritional supplements (SQ-LNS) to be evaluated as the markers of consumption for nutritional intervention studies. Forty-seven healthy women consumed a single supplement with either 8.6 mg of saccharin or 5 mg of trans-resveratrol, and urine was collected for 4 h. A rapid 11 min method employing multiple reaction monitoring and ultrahigh performance liquid chromatography coupled to a triple quadrupole mass spectrometer was developed to measure saccharin and resveratrol metabolites in urine simultaneously. The linear dynamic range of the method was from 3 to 1000 ng mL-1, with the correlation coefficient of 0.999 and limits of quantification from 15.28 to 53.03 ng mL-1. Sample preparation was simple dilution with an average recovery of 97.8%. Ion suppression was observed with urine concentrations >10%. Mean levels of saccharin and resveratrol-3-O-sulfate in urine were 5.481 ± 4.359 and 3.440 ± 4.160 nmol L-1, respectively. We developed and validated a method to measure saccharin and trans-resveratrol metabolites in urine to objectively corroborate the consumption of SQ-LNS for the first time in nutrition intervention studies.

Artificial sweeteners in non-alcoholic beverages: Occurrence and exposure estimation of the Portuguese population.

Artificial sweeteners such as acesulfame-potassium (ACE-K). saccharin (SAC), and aspartame (ASP), play a vital role in the food industry. Despite apparent benefits, several studies report adverse reactions on consumers. EFSA is currently re-evaluating several individual sweeteners, including ASP, Ace-K and SAC that shall be completed by 31 December 2020. Our goal was to evaluate, by liquid chromatography with ultraviolet detection (LC-UV), their levels in non-alcoholic beverages from the Portuguese market (soft drinks, sport drinks, energy drinks, and nectars), and estimate the exposure of the Portuguese adolescent/adult population. ACE-K was found in 85.7% of the samples, in mean levels of 97.4 mg/L. ASP and SAC, detected in 37.5% and 33.9% of the samples, were found in averages of 161.5 and 55.0 mg/L, respectively. The maximum limits set for ASP were exceeded in one energy drink. SAC exceeded the maximum permitted level (MPL) level in 3 soft drinks based on tea extracts. In 4 samples SAC was found but not mentioned in the label, and in one of these samples exceeded the MPL. The estimated daily intake (EDI), calculated in mg per kilogram of body weight per day, of ACE-K, SAC and ASP was found to be below the acceptable daily intake (ADI), both for Portuguese adolescents and adult population. Traditional soft drinks accounted for the highest EDIs representing 1.8%, 2.3% and 0.6% for ACE-K, SAC and ASP, respectively, of the ADI. Considering the previous report in Portugal it is observed that the population is currently exposed to a greater amount of artificial sweeteners, which may indicate a trend for more artificial sweeteners' usage in order to reduce sugar intake.

FTIR spectroscopy coupled with machine learning approaches as a rapid tool for identification and quantification of artificial sweeteners.

Fourier transform infrared (FTIR) spectroscopy calibrations were developed to simultaneously determine the multianalytes of five artificial sweeteners, including sodium cyclamate, sucralose, sodium saccharin, acesulfame-K and aspartame. By combining the pretreatment of the spectrum and principal component analysis, 131 feature wavenumbers were extracted from the full spectral range for modelling to qualitative and quantitative analysis. Compared to random forest, k nearest neighbour and linear discriminant analysis, support vector machine model had better predictivity, indicating the most effective identification performance. Furthermore, multivariate calibration models based on partial least squares regression were constructed for quantifying any combinations of the five artificial sweeteners, and validated by prediction data sets. As shown by the good agreement between the proposed method and the reference HPLC for the determination of the sweeteners in beverage samples, a promising and rapid tool based on FTIR spectroscopy, coupled with chemometrics, has been performed to identify and objectively quantify artificial sweeteners.

[Theoretical risk assessment for dietary exposure to sodium saccharin among residents in Nanjing City].

OBJECTIVE: To evaluate the potential risk of dietary exposure to sodium saccharin among residents in Nanjing City, and provide scientific evidence for safety surveillance and risk management in processed foods. METHODS: Based on the survey of dietary consumption of residents in Nanjing City, combining with the limits of sodium saccharin in processed foods(GB 2760-2014), using @Risk software to establish the cumulative dietary exposure in a probabilistic way, and compared with the acceptable daily intake(ADI) for risk assessment. RESULTS: The average exposure of sodium saccharin of residents was 0. 69 mg/kg, accounted for 13. 80% of ADI, while high exposure(P97. 5) was 5. 37 mg/kg, and accounted for 107. 36% of ADI. The exposure of sodium saccharin of residents in all age groups exceeded ADI were ranged from 20. 60% to 132. 80%. The intake of sodium saccharin exposure of high exposures(P97. 5) exceeded ADI was 132. 80% and 110. 75% in 18-49 years and 11-17 years people respectively. Cooked nuts, candied fruit and bean products were the main sources of sodium saccharin exposure compared with others. CONCLUSION: Dietary exposure assessment shows that the risk dietary exposure to sodium saccharin is generally safe. Residents who intake these processed foods higher should be paid more attention to reduce the level of sodium saccharin exposure.

Treatment of real sodium saccharin wastewater using multistage contact oxidation reactor and microbial community analysis.

In this study, multistage contact oxidation reactor (MCOR) with a novel carrier was used for treatment of high-strength sodium saccharin wastewater (SSW) under stepwise increasing salinities from 1.0% to 8.0%. The results revealed that MCOR could effectively remove the organic pollutants from SSW when influent salinity was no more than 4.5%; the chemical oxygen demand (COD) and NH4+-N removal efficiency under the optimal operating parameters ranged up to 91.5% and 92.7%, respectively. Microbial diversity analysis illustrated that the dominant microbes in SSW treatment system were substantially distinct at different salinities. Pseudomonas was predominant at salinity of 3.5%, while Marinobacterium (a species involved in COD removal) was enriched to a greater degree at salinity of 7.0%. CCA suggested that salinity was the main factor for dynamic evolutions of microbial community structures. This work demonstrated that MCOR is an appropriate method for the treatment of high-strength, high-salinity SSW.

Prevalence of ethanol and other potentially harmful excipients in pediatric oral medicines: survey of community pharmacies in a Nigerian City.

OBJECTIVE: Excipients are needed in the formulation of oral liquid medicines intended for children; they have however been reported to trigger safety issues. This study evaluated the concentrations and prevalence of ethanol and other potentially harmful excipients in pediatric formulations marketed in South Eastern Nigeria in line with international labeling guidelines and allowable daily limits (ADL). The study sampled oral pediatric formulations offered for sale in registered pharmacies. Those with accessible information leaflets were assessed for the presence and quantity of previously flagged excipients with potential to harm the pediatric population. RESULT: Of the 380 oral pediatric medicines, 140 provided access to list/quantity of ingredients. 47.9% (67) of the formulations contain at least one of the flagged excipients while the remaining only listed the active ingredients. Ethanol had the highest occurrence (62.7%) and was more in cough/cold medicines. A homeopathic cough and cold remedy had concentration of 90% v/v. Ethanol and sucrose in some formulations exhibited concentrations with a potential of crossing their approved daily intake (ADI) (1-90% v/v and 1.7 g-3.7 g/5 ml respectively). Ethanol use in studied pediatric formulations was quite high, with ethanol-containing formulations being prescribed for children 0-6 years and older. Only 26 (38.8%) completely satisfied the labelling requirements for ethanol containing formulations.

Photo-Fenton treatment of saccharin in a solar pilot compound parabolic collector: Use of olive mill wastewater as iron chelating agent, preliminary results.

The aim of this work was to investigate the treatment of the artificial sweetener saccharin (SAC) in a solar compound parabolic collector pilot plant by means of the photo-Fenton process at pH 2.8. Olive mill wastewater (OMW) was used as iron chelating agent to avoid acidification of water at pH 2.8. For comparative purposes, Ethylenediamine-N, N-disuccinic acid (EDDS), a well-studied iron chelator, was also employed at circumneutral pH. Degradation products formed along treatment were identified by LC-QTOF-MS analysis. Their degradation was associated with toxicity removal, evaluated by monitoring changes in the bioluminescence of Vibrio fischeri bacteria. Results showed that conventional photo-Fenton at pH 2.8 could easily degrade SAC and its intermediates yielding k, apparent reaction rate constant, in the range of 0.64-0.82 L kJ-1, as well as, eliminate effluent's chronic toxicity. Both OMW and EDDS formed iron-complexes able to catalyse H2O2 decomposition and generate HO. OMW yielded lower SAC oxidation rates (k = 0.05-0.1 L kJ-1) than EDDS (k = 2.21-7.88 L kJ-1) possibly due to its higher TOC contribution. However, the degradation rates were improved (k = 0.13 L kJ-1) by increasing OMW dilution in the reactant mixture. All in all, encouraging results were obtained by using OMW as iron chelating agent, thus rendering this approach promising towards the increase of process sustainability.

Applications of FT-NIRS combined with PLS multivariate methods for the detection & quantification of saccharin adulteration in commercial fruit juices.

Detection of adulteration in carbohydrate-rich foods like fruit juices is particularly difficult because of the variety of the commercial sweeteners available that match the concentration profiles of the major carbohydrates in the foods. In present study, a new sensitive and robust assay using Fourier Transform Near-Infrared Spectroscopy (FT-NIRS) combined with partial least square (PLS) multivariate methods has been developed for detection and quantification of saccharin adulteration in different commercial fruit juice samples. For this investigation, six different commercially available fruit juice samples were intentionally adulterated with saccharin at the following percentage levels: 0%, 0.10%, 0.30%, 0.50%, 0.70%, 0.90%, 1.10%, 1.30%, 1.50%, 1.70% and 2.00% (weight/volume). Altogether, 198 samples were used including 18 pure juice samples (unadulterated) and 180 juice samples adulterated with saccharin. PLS multivariate methods including partial least-squares discriminant analysis (PLS-DA) and partial least-squares regressions (PLSR) were applied to the obtained spectral data to build models. The PLS-DA model was employed to differentiate between pure fruit juice samples and those adulterated with saccharin. The R2 value obtained for the PLS-DA model was 97.90% with an RMSE error of 0.67%. Similarly, a PLS regression model was also developed to quantify the amount of saccharin adulterant in juice samples. The R2 value obtained for the PLSR model was 97.04% with RMSECV error of 0.88%. The employed model was then cross-validated by using a test set which included 30% of the total adulterated juice samples. The excellent performance of the model was proved by the low root mean squared error of prediction value of 0.92% and the high correlation factor of 0.97. This newly developed method is robust, nondestructive, highly sensitive and economical.

High-throughput quantification of sodium saccharin in foods by ambient flame ionization mass spectrometry.

Ambient flame ionization (AFI) coupled with triple quadrupole tandem mass spectrometry was developed for quantitative analysis of sodium saccharin (SAC) in various food samples. Typically, the micro-flame by the combustion of n-butane provided a heating zone for fast desorption and ionization of analytes in milliseconds. Then high ion abundance of analyte could be produced in a short time, which made AFI-MS possess a very high sensitivity for SAC detection and was particularly appropriate for the quantification in multiple reaction monitor (MRM) mode. Liquid samples were introduced into outer flame using dip-it tips in order to facilitate a rapid and high-throughput analysis. Saccharin-d4 was used as the internal standard to compensate for the variations of the ion intensities. With a minimal sample preparation, a linear range of 4-100 µg/mL was developed with all linear relationships of different matrices (including coke, juice, liquors, sunflower seeds and sweetmeats) greater than 0.992. Recoveries for coke and apple matrices were ranged from 88.4% to 108.9% at the concentration of 5, 20, 80 µg/mL and the limits of detection (LODs) were in the range of 0.12-0.21 µg/mL. Furthermore, the feasibility of this method was exhibited by the quantification analysis of SAC in seventeen real samples. These results indicated that AFI-MS was a valuable strategy for rapid screening detection and precise quantification analysis of SAC in food.

Development of a Sequential Injection Analysis System for the Determination of Saccharin.

Saccharin is a powerfully sweet nonnutritive sweetener that has been approved for food-processing applications within the range of 100-1200 mg/kg. A simple, rapid, and cost-effective sequential injection analysis (SIA) technique was developed to determine the saccharin level. This method is based on the reaction of saccharin with p-chloranil in an ethanol medium with a hydrogen peroxide (H2O2) acceleration, and the resultant violet-red compound was detected using a UV-Vis spectrophotometer at λmax = 420 nm. To ascertain the optimal conditions for the SIA system, several parameters were investigated, including buffer flow rate and volume, p-chloranil concentration, and reactant volumes (saccharin, p-chloranil, and H2O2). The optimum setup of the SIA system was achieved with a buffer flow rate, buffer volume, and draw-up time of 1.2 mL/min, 2900 µL, and ~145 s, respectively. The optimal p-chloranil concentration is 30 mM, and the best reactant volumes, presented in an ordered sequence, are as follows: 30 µL of H2O2, 450 µL of saccharin, and 150 µL of p-chloranil. The optimized SIA configuration produced a good linear calibration curve with a correlation coefficient (R² = 0.9812) in the concentration range of 20-140 mg/L and with a detection limit of 19.69 mg/L. Analytical applications in different food categories also showed acceptable recovery values in the range of 93.1-111.5%. This simple and rapid SIA system offers great feasibility for the saccharin quality control in food-product processing.