Background Aquaculture water plays an important role in the dissemination of antibiotic-resistant bacteria during harvest of shrimps. Mitigation of bacteria through discharge is essential to prevent dissemination downstream. Chemical disinfection of culture water is feasible compared to other methods of bacterial inactivation. Objective To study the effect of different disinfectant agent’s viz., chlorine, Fenton’s reagent, and hydrogen peroxide (H2O2) on inactivation of bacteria from shrimp pond water Methods The water samples were subjected to treatment with various concentrations of chlorine (0.0, 1.0, 2.5, 5.0 and 10.0 mg L−1), Fenton’s reagent (1:10 mM ratio of Fe2+:H2O2; 2:20, 3:30, 4:40, 5:50) and H2O2 (20, 30, 40 and 50 mM) for different time durations (5 min, 15 min, 30 min and 60 min). Results The results indicated that all the disinfecting agents inactivated both the total heterotrophic bacteria and tetracycline-resistant bacteria with increased concentrations and time. At the end of 60 min treatment with chlorination (2.5 mg Cl2 L−1), Fenton’s reagent (2 mM Fe2+ + 20 mM H2O2) and H2O2 (50 mM H2O2), the total heterotrophic bacterial count in the water samples gradually decreased by 2.35, 2.65, and 1.38 log10 CFU mL−1, and tetracycline-resistant bacteria count reduced by 1.57, 1.66, and 1.43 log10 CFU mL−1, respectively from initial bacterial load. Conclusions The study revealed that disinfection agents can be successfully employed in the inactivation of antibiotic-resistant bacteria discharged through aquaculture water. Among three disinfection agents, Fenton’s reagent has been found effective in inhibiting both heterotrophic bacteria and tetracycline-resistant bacteria from water samples. Highlights Bacterial inactivation studies were carried with Chlorination, Fenton’s reagent, and Hydrogen peroxide. The highest decrease in HPC (2.65 log) and tetracycline-resistant bacterial (1.66 log) was noticed in the water samples treated with Fenton’s reagent. The use of disinfection agents effectively mitigates antibiotic-resistant bacteria from aquaculture wastewater.
{"title":"Bacterial Inactivation Studies in Shrimp Pond Water by using Different Disinfectant Agents","authors":"Ranjit Kumar Nadella, Satyen Kumar Panda, Devananda Uchio, Pankaj Kishore, Madhu V.R, Minimol Vallamattath Ayyappan, Madhusudana Rao Badireddy, Pani Prasad Kuricheti, Ram Prakash Raman, Mukteswar Prasad Mothadaka","doi":"10.1093/jaoacint/qsae073","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae073","url":null,"abstract":"Background Aquaculture water plays an important role in the dissemination of antibiotic-resistant bacteria during harvest of shrimps. Mitigation of bacteria through discharge is essential to prevent dissemination downstream. Chemical disinfection of culture water is feasible compared to other methods of bacterial inactivation. Objective To study the effect of different disinfectant agent’s viz., chlorine, Fenton’s reagent, and hydrogen peroxide (H2O2) on inactivation of bacteria from shrimp pond water Methods The water samples were subjected to treatment with various concentrations of chlorine (0.0, 1.0, 2.5, 5.0 and 10.0 mg L−1), Fenton’s reagent (1:10 mM ratio of Fe2+:H2O2; 2:20, 3:30, 4:40, 5:50) and H2O2 (20, 30, 40 and 50 mM) for different time durations (5 min, 15 min, 30 min and 60 min). Results The results indicated that all the disinfecting agents inactivated both the total heterotrophic bacteria and tetracycline-resistant bacteria with increased concentrations and time. At the end of 60 min treatment with chlorination (2.5 mg Cl2 L−1), Fenton’s reagent (2 mM Fe2+ + 20 mM H2O2) and H2O2 (50 mM H2O2), the total heterotrophic bacterial count in the water samples gradually decreased by 2.35, 2.65, and 1.38 log10 CFU mL−1, and tetracycline-resistant bacteria count reduced by 1.57, 1.66, and 1.43 log10 CFU mL−1, respectively from initial bacterial load. Conclusions The study revealed that disinfection agents can be successfully employed in the inactivation of antibiotic-resistant bacteria discharged through aquaculture water. Among three disinfection agents, Fenton’s reagent has been found effective in inhibiting both heterotrophic bacteria and tetracycline-resistant bacteria from water samples. Highlights Bacterial inactivation studies were carried with Chlorination, Fenton’s reagent, and Hydrogen peroxide. The highest decrease in HPC (2.65 log) and tetracycline-resistant bacterial (1.66 log) was noticed in the water samples treated with Fenton’s reagent. The use of disinfection agents effectively mitigates antibiotic-resistant bacteria from aquaculture wastewater.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"209 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268352","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-18DOI: 10.1093/jaoacint/qsae072
Natália Sabina dos Santos Galvão, Ana Carolina Kogawa
Background Ivermectin (IVE), a broad-spectrum antiparasitic, is used in human and animal health. Analytical methods for evaluating IVE in pharmaceutical products are found in the literature and in official compendiums. However, the vast majority of them do not have an eco-friendly approach. Objective and Method The aim of this review is to present an overview of existing analytical methods for evaluating IVE in pharmaceutical matrices in the context of Green Analytical Chemistry (GAC) and show possibilities for increasing their greenness. Results GAC is a current alternative to promote sustainable development in laboratories and chemical-pharmaceutical industries, therefore, through its principles, such as reducing the use of aggressive solvents, it is possible to make processes more ecological. However, the vast majority of analytical methods available in the literature and official compendiums do not present an eco-friendly approach. 70% of the methods are by HPLC. Among the various pharmaceutical matrices, the most evaluated are tablets (37%). Of all the solvents used in HPLC, UPLC, HPLC-MS/MS, UV and TLC methods, the combination of methanol and acetonitrile is the most chosen, accounting for more than 50% of occurrences. Conclusions Analytical methods for evaluating IVE-based products can be leveraged within the scope of GAC, bringing sustainable work opportunities to analytical development laboratories around the world. Highlights This review shows an overview of the analytical methods present in the literature and official compendiums to evaluate pharmaceutical IVE matrices, in the context of green analytical chemistry.
{"title":"Ivermectin-based products in the context of green pharmaceutical analysis","authors":"Natália Sabina dos Santos Galvão, Ana Carolina Kogawa","doi":"10.1093/jaoacint/qsae072","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae072","url":null,"abstract":"Background Ivermectin (IVE), a broad-spectrum antiparasitic, is used in human and animal health. Analytical methods for evaluating IVE in pharmaceutical products are found in the literature and in official compendiums. However, the vast majority of them do not have an eco-friendly approach. Objective and Method The aim of this review is to present an overview of existing analytical methods for evaluating IVE in pharmaceutical matrices in the context of Green Analytical Chemistry (GAC) and show possibilities for increasing their greenness. Results GAC is a current alternative to promote sustainable development in laboratories and chemical-pharmaceutical industries, therefore, through its principles, such as reducing the use of aggressive solvents, it is possible to make processes more ecological. However, the vast majority of analytical methods available in the literature and official compendiums do not present an eco-friendly approach. 70% of the methods are by HPLC. Among the various pharmaceutical matrices, the most evaluated are tablets (37%). Of all the solvents used in HPLC, UPLC, HPLC-MS/MS, UV and TLC methods, the combination of methanol and acetonitrile is the most chosen, accounting for more than 50% of occurrences. Conclusions Analytical methods for evaluating IVE-based products can be leveraged within the scope of GAC, bringing sustainable work opportunities to analytical development laboratories around the world. Highlights This review shows an overview of the analytical methods present in the literature and official compendiums to evaluate pharmaceutical IVE matrices, in the context of green analytical chemistry.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"33 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268353","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-14DOI: 10.1093/jaoacint/qsae071
Fereidoun Forghani, Eni Themeli, Tam Mai, Mansour Samadpour
Background There is a high demand in food industry and public health for rapid automated methods capable of high volume sample processing. Objective In an unpaired study Roka Atlas® System performance was compared with Health Canada reference method MFHPB-30 for Listeria spp. (LSP Roka assay) and Listeria monocytogenes (LmG2 Roka Assay) detection on plastic (PL), sealed concrete (SC), and stainless steel (SS) surfaces (45 samples each per candidate or reference method). Methods Seeking shorter enrichment time for the candidate method, R2 medium pre-enrichment for 14, 16, and 24 h at 35 °C was combined with the Roka assay. Listeria welshimeri, L. innocua, and L. monocytogenes were employed to individually inoculate each of the three surfaces, with two competing microorganisms within the 10–100 fold higher concentration range. Results False negative, false positive, sensitivity and specificity were 0, 0, 100, and 100%, respectively, for the plastic, sealed concrete, and stainless steel surfaces, regardless of inoculation level (high, low, and uninoculated) and enrichment time. Candidate method detected 10, 7 and 9 true positives, versus 10, 6 and 10 by the reference method in individually inoculated SS, PL and SC, respectively. Conclusion Probability of detection for all the three surfaces for the Roka Atlas® System was comparable to the reference method, in this unpaired study. Highlights The Roka Atlas® System detected targets after as little as 14 h enrichment. Surface type did not negatively affect assay sensitivity or specificity. The Roka Atlas® System was comparable to the reference method.
{"title":"Comparison of Roka Atlas® System Performance and Health Canada Reference Method for Listeria Detection from Plastic, Sealed Concrete, and Stainless Steel Surface Samples","authors":"Fereidoun Forghani, Eni Themeli, Tam Mai, Mansour Samadpour","doi":"10.1093/jaoacint/qsae071","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae071","url":null,"abstract":"Background There is a high demand in food industry and public health for rapid automated methods capable of high volume sample processing. Objective In an unpaired study Roka Atlas® System performance was compared with Health Canada reference method MFHPB-30 for Listeria spp. (LSP Roka assay) and Listeria monocytogenes (LmG2 Roka Assay) detection on plastic (PL), sealed concrete (SC), and stainless steel (SS) surfaces (45 samples each per candidate or reference method). Methods Seeking shorter enrichment time for the candidate method, R2 medium pre-enrichment for 14, 16, and 24 h at 35 °C was combined with the Roka assay. Listeria welshimeri, L. innocua, and L. monocytogenes were employed to individually inoculate each of the three surfaces, with two competing microorganisms within the 10–100 fold higher concentration range. Results False negative, false positive, sensitivity and specificity were 0, 0, 100, and 100%, respectively, for the plastic, sealed concrete, and stainless steel surfaces, regardless of inoculation level (high, low, and uninoculated) and enrichment time. Candidate method detected 10, 7 and 9 true positives, versus 10, 6 and 10 by the reference method in individually inoculated SS, PL and SC, respectively. Conclusion Probability of detection for all the three surfaces for the Roka Atlas® System was comparable to the reference method, in this unpaired study. Highlights The Roka Atlas® System detected targets after as little as 14 h enrichment. Surface type did not negatively affect assay sensitivity or specificity. The Roka Atlas® System was comparable to the reference method.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"1 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268354","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-09DOI: 10.1093/jaoacint/qsae070
Isaac Lee, Quanyin Gao, Wei Liu, Darshan Patel, Malissa Smith, Hong You, Tushar Patel, Karine Aylozyan, Silva Babajanian, Teddy Collins, Darryl Sullivan, Peter Chang, Gary Swanson
Background A multi-laboratory validation study was performed on AOAC Official Method of Analysis (OMA) 2016.09, for final action. Eight different laboratories throughout the world participated in the study tested the same set of 6 different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria. Objective The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, limit of detection (LOD), and limit of quantitation (LOQ) by multiple laboratories to satisfy the requirement of moving the OMA 2016.09 to the final action status. Accuracy and ruggedness were already validated in earlier work of single laboratory validation (1), and it was not necessary to include these validation parameters in the multi-laboratory validation study. Method Laboratory samples containing Aloe were sent out to participating laboratories. Each lab followed AOAC 2016.09 (First Action status) to analyze contents of aloin A, aloin B, and aloe emodin using high performance liquid chromatography (HPLC) instrument. The results generated by each laboratory were collected and evaluated. Results The specificity results show that blank and matrix chromatograms do not contain major interfering peaks on the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion (ppb), 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) value of ≥ 0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The limit of detection (LOD) results show that the signal-to-noise (S/N) ratio of 10 ppb standards for all three components are about 3. The limit of quantitation (LOQ) results show that the S/N ratio of 20 ppb standards for all three components are about 10. Conclusions The validation parameters (specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ) have been successfully analyzed, and it shows that the test method is suitable for its intended use. Highlights The test method has been successfully validated by the eight different laboratories around the world (US, UK, Germany, and Canada). Each of the laboratory is managed independently by the site lab management team. This multi-lab study validated the method of Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using high performance liquid chromatography (HPLC), and the method fits for its intended purpose.
{"title":"Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using HPLC Multi-Laboratory Validation Study, AOAC 2016.09, Final Action Status","authors":"Isaac Lee, Quanyin Gao, Wei Liu, Darshan Patel, Malissa Smith, Hong You, Tushar Patel, Karine Aylozyan, Silva Babajanian, Teddy Collins, Darryl Sullivan, Peter Chang, Gary Swanson","doi":"10.1093/jaoacint/qsae070","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae070","url":null,"abstract":"Background A multi-laboratory validation study was performed on AOAC Official Method of Analysis (OMA) 2016.09, for final action. Eight different laboratories throughout the world participated in the study tested the same set of 6 different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria. Objective The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, limit of detection (LOD), and limit of quantitation (LOQ) by multiple laboratories to satisfy the requirement of moving the OMA 2016.09 to the final action status. Accuracy and ruggedness were already validated in earlier work of single laboratory validation (1), and it was not necessary to include these validation parameters in the multi-laboratory validation study. Method Laboratory samples containing Aloe were sent out to participating laboratories. Each lab followed AOAC 2016.09 (First Action status) to analyze contents of aloin A, aloin B, and aloe emodin using high performance liquid chromatography (HPLC) instrument. The results generated by each laboratory were collected and evaluated. Results The specificity results show that blank and matrix chromatograms do not contain major interfering peaks on the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion (ppb), 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) value of ≥ 0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The limit of detection (LOD) results show that the signal-to-noise (S/N) ratio of 10 ppb standards for all three components are about 3. The limit of quantitation (LOQ) results show that the S/N ratio of 20 ppb standards for all three components are about 10. Conclusions The validation parameters (specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ) have been successfully analyzed, and it shows that the test method is suitable for its intended use. Highlights The test method has been successfully validated by the eight different laboratories around the world (US, UK, Germany, and Canada). Each of the laboratory is managed independently by the site lab management team. This multi-lab study validated the method of Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using high performance liquid chromatography (HPLC), and the method fits for its intended purpose.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"37 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142192522","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-01Epub Date: 2022-04-27DOI: 10.1177/10598405221094282
Kyung-Ah Kang, Shin-Jeong Kim, SoRa Kang, JungMin Lee
This study aimed to investigate the effects of a violence-prevention education program using empathy (VPEP-E) on elementary school students. This quasi-experimental design examined fifth-grade students' (a) empathy level, (b) perception of violence, and (c) permissive and negligent attitudes toward violence, using a pre- and post-test design. A total of 101 students participated: the experimental group (n = 48) received eight sessions of VPEP-E, whereas the control group (n = 53) received violence prevention education through classroom lectures. Significant differences were observed between the groups' empathy level (t = 6.81, p < .001), perception of violence (t = 2.79, p = .006), and permissive and negligent attitudes toward violence (t = -2.21, p = .030; t = -2.02, p = .046). Thus, a school-based VPEP-E may help elementary school students. Long-term studies evaluating behavioral changes from VPEP-E implementation are needed for establishing the effects on violent behavior.
{"title":"Effects of a Violence Prevention Education Program Using Empathy (VPEP-E) on Fifth-Grade Students in South Korea.","authors":"Kyung-Ah Kang, Shin-Jeong Kim, SoRa Kang, JungMin Lee","doi":"10.1177/10598405221094282","DOIUrl":"10.1177/10598405221094282","url":null,"abstract":"<p><p>This study aimed to investigate the effects of a violence-prevention education program using empathy (VPEP-E) on elementary school students. This quasi-experimental design examined fifth-grade students' (a) empathy level, (b) perception of violence, and (c) permissive and negligent attitudes toward violence, using a pre- and post-test design. A total of 101 students participated: the experimental group (<i>n</i> = 48) received eight sessions of VPEP-E, whereas the control group (<i>n</i> = 53) received violence prevention education through classroom lectures. Significant differences were observed between the groups' empathy level (<i>t</i> = 6.81, <i>p</i> < .001), perception of violence (<i>t</i> = 2.79, <i>p</i> = .006), and permissive and negligent attitudes toward violence (<i>t</i> = -2.21, <i>p</i> = .030; <i>t</i> = -2.02, <i>p</i> = .046). Thus, a school-based VPEP-E may help elementary school students. Long-term studies evaluating behavioral changes from VPEP-E implementation are needed for establishing the effects on violent behavior.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"59 1","pages":"361-371"},"PeriodicalIF":1.5,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83363633","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-26DOI: 10.1093/jaoacint/qsae064
Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise
Background The National Institute of Standards and Technology (NIST) has produced over 40 botanical dietary supplement Standard Reference Materials® (SRMs) and reference materials (RMs) with values assigned for chemical markers and/or active compounds. Although environmental accumulation or inadvertent introduction of toxic elements (arsenic, cadmium, lead, and mercury) is a potential source of exposure in botanical dietary supplement products, the majority of the dietary supplement SRMs/RMs do not have values assigned for the four major toxic elements. Objective To determine As, Cd, Pb, and Hg content in the current inventory of NIST botanical dietary supplement SRMs/RMs. Methods Fifteen SRMs/RMs suites of plant part, extract, and finished products [i.e., solid oral dosage form (SODF)] were analyzed for As, Cd, Pb, and Hg using nitric acid microwave-assisted digestion followed by quantification using inductively coupled plasma—mass spectrometry. Results Results for control samples were in good agreement with certified values indicating that the analyses of 38 individual botanical SRMs/RMs were in control. Characterization of linked plant/extract SRMs/RMs derived from the same source materials demonstrated that while extraction processes can often yield extracts with lower toxic element content for Hg or As, it is also possible for mass fraction levels to remain unchanged or even increase following extraction. Conclusion The results fill significant knowledge gaps in toxic element content ranges for SRMs/RMs where no NIST assigned values existed, in particular for Hg content and for extract and SODF matrices. With comprehensive toxic element content now available, researchers can better select appropriate dietary supplement SRMs/RMs for use as controls in the analysis of dietary supplement ingredients and products. Highlights Results for As, Cd, Pb, and Hg are reported for 38 dietary supplement SRMs/RMs including 6 suites of plant, extract, and SODF and 9 pairs of plant and extract from the same batch of plant material.
{"title":"Determination of Toxic Elements in Botanical Dietary Supplement Ingredient Reference Materials","authors":"Jennifer Fong Sam, Adam J Kuszak, Patrick J Gray, Stephen A Wise","doi":"10.1093/jaoacint/qsae064","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae064","url":null,"abstract":"Background The National Institute of Standards and Technology (NIST) has produced over 40 botanical dietary supplement Standard Reference Materials® (SRMs) and reference materials (RMs) with values assigned for chemical markers and/or active compounds. Although environmental accumulation or inadvertent introduction of toxic elements (arsenic, cadmium, lead, and mercury) is a potential source of exposure in botanical dietary supplement products, the majority of the dietary supplement SRMs/RMs do not have values assigned for the four major toxic elements. Objective To determine As, Cd, Pb, and Hg content in the current inventory of NIST botanical dietary supplement SRMs/RMs. Methods Fifteen SRMs/RMs suites of plant part, extract, and finished products [i.e., solid oral dosage form (SODF)] were analyzed for As, Cd, Pb, and Hg using nitric acid microwave-assisted digestion followed by quantification using inductively coupled plasma—mass spectrometry. Results Results for control samples were in good agreement with certified values indicating that the analyses of 38 individual botanical SRMs/RMs were in control. Characterization of linked plant/extract SRMs/RMs derived from the same source materials demonstrated that while extraction processes can often yield extracts with lower toxic element content for Hg or As, it is also possible for mass fraction levels to remain unchanged or even increase following extraction. Conclusion The results fill significant knowledge gaps in toxic element content ranges for SRMs/RMs where no NIST assigned values existed, in particular for Hg content and for extract and SODF matrices. With comprehensive toxic element content now available, researchers can better select appropriate dietary supplement SRMs/RMs for use as controls in the analysis of dietary supplement ingredients and products. Highlights Results for As, Cd, Pb, and Hg are reported for 38 dietary supplement SRMs/RMs including 6 suites of plant, extract, and SODF and 9 pairs of plant and extract from the same batch of plant material.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"30 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141785253","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-30DOI: 10.1093/jaoacint/qsae039
Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz
Background Products containing humic acids (HA) and fulvic acids (FA) have significant commercial potential, however, unknown to the consumer, some products may be mislabeled or contain adulterants. The prevalence of mislabelling and adulterants is primarily found in FA products. Using UV-Vis spectroscopy to differentiate between real and fake FA products is practical and desirable. Objective The objective of this study was to expand the data set generated using a UV-VIS based method proposed by Mayhew et al., 2023. Methods In total, thirty (30) test samples were used to generate ninety test portions (3 replicates per test sample) for analysis using the UV-Vis methodology outlined in Mayhew et al., 2023, which in this study is referred to as the UVAC (UV absorbance confirmation) method. Results None of the thirteen FA test samples investigated were determined as humified using the UVAC method. The FA samples studied comprised of two IHSS standards, five commercial FA products (CFAP) and six full FA fractions (SFA), which were isolated from six known solid humic material sources (SHMS). There was a leonardite, a humalite, and four peat sources used as the SHMS. Analysis of the neutralized extract of the SHMS found only 3/6 SHMS were determined as humified. Six HA (SHA) test samples were also generated by isolating the HA from the SHMS and only 3/6 SHA were determined as humified. Conclusion Given the high prevalence of false determinations more work is needed to improve the method so it can be used by industry or regulators. Highlights The proposed method failed to determine IHSS FA standards as humified. Although the method is practical, it needs improvement and further study before it can be used for reliable differentiation of real from fake FA or HA.
背景 含腐植酸（HA）和富里酸（FA）的产品具有巨大的商业潜力，然而，消费者并不知道，有些产品可能贴错标签或含有掺假物。贴错标签和掺假的情况主要出现在富里酸产品中。使用紫外可见光谱来区分真假 FA 产品既实用又可取。本研究的目的是扩大使用 Mayhew 等人 2023 年提出的基于紫外可见光谱的方法生成的数据集。方法 使用 Mayhew 等人，2023 年提出的紫外-可见光方法（在本研究中称为 UVAC（紫外吸光度确认）方法），总共使用了三十（30）个测试样本来生成九十个测试部分（每个测试样本 3 个重复）进行分析。结果 在所调查的 13 个 FA 测试样品中，没有一个样品被确定为使用紫外吸光度确认法进行的腐殖化。所研究的 FA 样品包括两种 IHSS 标准、五种商业 FA 产品 (CFAP) 和六种全 FA 馏分 (SFA)，它们是从六种已知的固体腐殖质材料来源 (SHMS) 中分离出来的。其中有一种柠檬岩、一种腐植岩和四种泥炭来源被用作 SHMS。对 SHMS 的中和提取物进行分析后发现，只有 3/6 的 SHMS 被确定为腐殖质。通过分离 SHMS 中的 HA，还生成了 6 个 HA（SHA）测试样本，结果只有 3/6 的 SHA 被确定为腐殖化。结论 鉴于错误测定的发生率较高，需要进一步改进该方法，以便供行业或监管机构使用。要点 建议的方法未能确定 IHSS FA 标准为腐殖化。虽然该方法很实用，但还需要改进和进一步研究，才能用于可靠地区分真假 FA 或 HA。
{"title":"Evaluating the use of UV Absorbance for the Differentiation of Humified from Non-humified Materials","authors":"Mohammad Rahbari, Jarrod Psutka, Richard Lamar, Fernando Rosario-Ortiz","doi":"10.1093/jaoacint/qsae039","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae039","url":null,"abstract":"Background Products containing humic acids (HA) and fulvic acids (FA) have significant commercial potential, however, unknown to the consumer, some products may be mislabeled or contain adulterants. The prevalence of mislabelling and adulterants is primarily found in FA products. Using UV-Vis spectroscopy to differentiate between real and fake FA products is practical and desirable. Objective The objective of this study was to expand the data set generated using a UV-VIS based method proposed by Mayhew et al., 2023. Methods In total, thirty (30) test samples were used to generate ninety test portions (3 replicates per test sample) for analysis using the UV-Vis methodology outlined in Mayhew et al., 2023, which in this study is referred to as the UVAC (UV absorbance confirmation) method. Results None of the thirteen FA test samples investigated were determined as humified using the UVAC method. The FA samples studied comprised of two IHSS standards, five commercial FA products (CFAP) and six full FA fractions (SFA), which were isolated from six known solid humic material sources (SHMS). There was a leonardite, a humalite, and four peat sources used as the SHMS. Analysis of the neutralized extract of the SHMS found only 3/6 SHMS were determined as humified. Six HA (SHA) test samples were also generated by isolating the HA from the SHMS and only 3/6 SHA were determined as humified. Conclusion Given the high prevalence of false determinations more work is needed to improve the method so it can be used by industry or regulators. Highlights The proposed method failed to determine IHSS FA standards as humified. Although the method is practical, it needs improvement and further study before it can be used for reliable differentiation of real from fake FA or HA.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"23 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140831635","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC identified the need for a reliable confirmatory screening method. Such qualitative approach is required for compliance checking and to support product release in manufacturing. Objective Data were collected from 5 independent laboratories that applied the AOAC Official First Action Method AOAC 2020.04 to demonstrate adequate performance under reproducibility conditions. Probability of Detection (POD) was calculated in blank test samples and test samples spiked at the Screening Target Concentration (STC) level, with the objective to achieve PODs ≤ 10% and ≥ 90%, respectively. Additionally, the effectiveness of the screening method was assessed through participation to 92 proficiency test samples. Methods Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals and baby foods) and other ingredients such as eggs, animal fat and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (Stream A); 23 Beta-lactams (Stream B); 14 Aminoglycosides (Stream C) and 10 Tetracyclines (Stream D). Results The multi-laboratory validation led to PODs at the STC ≥ 94% and PODs in the blank ≤ 9%. Further application of the multi-laboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). Conclusion The inter-laboratory reproducibility determined for this method met the acceptance criteria defined in AOAC SMPR 2018.010. Highlights AOAC has approved the method for Final Action Status.
{"title":"Screening of 152 Veterinary Drug Residues in Animal Source Foods by LC-MS/MS, Multilaboratory Validation Study: Final Action 2020.04","authors":"Aurélien Desmarchelier, Thomas Bessaire, Marie-Claude Savoy, Adrienne Tarres, Claudia Mujahid, Andrea Beck, Pascal Mottier, Xun Fu, Wai-Chinn Chan, Stéphanie Laborie, Nadine Hagenbourgerr, Gislaine Miranda, Thierry Delatour","doi":"10.1093/jaoacint/qsae032","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae032","url":null,"abstract":"Background The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC identified the need for a reliable confirmatory screening method. Such qualitative approach is required for compliance checking and to support product release in manufacturing. Objective Data were collected from 5 independent laboratories that applied the AOAC Official First Action Method AOAC 2020.04 to demonstrate adequate performance under reproducibility conditions. Probability of Detection (POD) was calculated in blank test samples and test samples spiked at the Screening Target Concentration (STC) level, with the objective to achieve PODs ≤ 10% and ≥ 90%, respectively. Additionally, the effectiveness of the screening method was assessed through participation to 92 proficiency test samples. Methods Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals and baby foods) and other ingredients such as eggs, animal fat and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (Stream A); 23 Beta-lactams (Stream B); 14 Aminoglycosides (Stream C) and 10 Tetracyclines (Stream D). Results The multi-laboratory validation led to PODs at the STC ≥ 94% and PODs in the blank ≤ 9%. Further application of the multi-laboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). Conclusion The inter-laboratory reproducibility determined for this method met the acceptance criteria defined in AOAC SMPR 2018.010. Highlights AOAC has approved the method for Final Action Status.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"161 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140609396","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-15DOI: 10.1093/jaoacint/qsae034
Hany H Monir, Heba A Mohamed, Amr M Badawy, Marianne Nebsen, Christine K Nessim
Background Through the use of sustainable and green chemistry concepts, scientists need to decrease waste, conserve energy, and develop safe substitutes for hazardous compounds, all for protecting and benefiting society and the environment. Objective Four novel eco-friendly ion selective electrodes (ISE) were created to determine Ethamsylate (ETM) in bulk powder and different pharmaceutical formulations. The present electrodes were fabricated and evaluated to clearly distinguish ETM from a variety of inorganic, organic ions, sugars, some common drug excipients and the degradation product, hydroquinone (HQ) of ETM, and thus could be used for stability-indicating methods. Methods The electrodes fabrication was based on 2-nitrophenyl octyl ether (NPOE) that was employed as a plasticizer in electrodes 1, 2, and 3 within a polymeric matrix of polyvinyl chloride (PVC) except for electrode 4, in which dibutyl sebacate was used as a plasticizer. Electrodes 1 & 2 were fabricated using tetra dodecyl ammonium bromide as an anionic exchanger and adding 4-sulfocalix-8-arene as an ionophore only to electrode 2, but electrode 1 prepared without incorporation of an ionophore. The fabrication of electrodes 3 & 4 was based on ethamsylate-tetraphenylborate (ETM-TPB) as an ion-association complex in a PVC matrix. The environmental sustainability was assessed using Green Analytical Procedure Index (GAPI), and Analytical Greenness Metric for Sample Preparation (AGREEprep). Results Electrodes 1 & 2 had linear dynamic ranges of (10−1—10 −5) and (10−1—10 −4) respectively, with a Nernstian slope of 49.6 and 53.2 mV/decade, respectively. Electrodes 3 & 4 had linear dynamic ranges of (10−1—10 −4), with a Nernstian slope of 43.9 and 40.2 mV/decade, respectively. Conclusion The generated electrodes' selectivity coefficients showed good selectivity for ETM. The utility 4-sulfocalix-8-arene as ionophore had a significant influence on increasing the membrane sensitivity and selectivity of electrode 2 compared to other electrodes.
{"title":"Enhancing the Sustainability of Eco-friendly Potentiometric Ion Selective Electrodes for Stability-Indicating Measurement of Ethamsylate: Application in Bulk and Pharmaceutical Formulations","authors":"Hany H Monir, Heba A Mohamed, Amr M Badawy, Marianne Nebsen, Christine K Nessim","doi":"10.1093/jaoacint/qsae034","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae034","url":null,"abstract":"Background Through the use of sustainable and green chemistry concepts, scientists need to decrease waste, conserve energy, and develop safe substitutes for hazardous compounds, all for protecting and benefiting society and the environment. Objective Four novel eco-friendly ion selective electrodes (ISE) were created to determine Ethamsylate (ETM) in bulk powder and different pharmaceutical formulations. The present electrodes were fabricated and evaluated to clearly distinguish ETM from a variety of inorganic, organic ions, sugars, some common drug excipients and the degradation product, hydroquinone (HQ) of ETM, and thus could be used for stability-indicating methods. Methods The electrodes fabrication was based on 2-nitrophenyl octyl ether (NPOE) that was employed as a plasticizer in electrodes 1, 2, and 3 within a polymeric matrix of polyvinyl chloride (PVC) except for electrode 4, in which dibutyl sebacate was used as a plasticizer. Electrodes 1 & 2 were fabricated using tetra dodecyl ammonium bromide as an anionic exchanger and adding 4-sulfocalix-8-arene as an ionophore only to electrode 2, but electrode 1 prepared without incorporation of an ionophore. The fabrication of electrodes 3 & 4 was based on ethamsylate-tetraphenylborate (ETM-TPB) as an ion-association complex in a PVC matrix. The environmental sustainability was assessed using Green Analytical Procedure Index (GAPI), and Analytical Greenness Metric for Sample Preparation (AGREEprep). Results Electrodes 1 & 2 had linear dynamic ranges of (10−1—10 −5) and (10−1—10 −4) respectively, with a Nernstian slope of 49.6 and 53.2 mV/decade, respectively. Electrodes 3 & 4 had linear dynamic ranges of (10−1—10 −4), with a Nernstian slope of 43.9 and 40.2 mV/decade, respectively. Conclusion The generated electrodes' selectivity coefficients showed good selectivity for ETM. The utility 4-sulfocalix-8-arene as ionophore had a significant influence on increasing the membrane sensitivity and selectivity of electrode 2 compared to other electrodes.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"462 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140609397","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-13DOI: 10.1093/jaoacint/qsae031
Denis Cuany, Sean Austin
Background We previously published a method for the determination of β-Galactooligosaccharides (GOS) in Infant Formula and Adult Nutritionals which is currently First Action AOAC Method 2021.01. In this study, reproducibility data were collected to support the promotion of the method to Final Action. Method A collaborative study was organized, to which 14 laboratories from eight different countries participated. Initially, laboratories were requested to analyze two practice samples and request guidance from the study director in case of issues. Successful laboratories proceeded to analyze seven samples (six infant formula and one adult nutritional) received as blind duplicates. Results Thirteen laboratories reported acceptable results for practice sample 1. Practice sample 2 could only be delivered to eight of the laboratories due to restrictions at customs. The 13 laboratories successfully analyzing practice sample 1 were requested to continue with the analysis of the MLT samples. Laboratory 14 was unable to solve some technical difficulties, so their data could not be used. Out of the seven samples tested, results for six infant formula met the requirements of the AOAC SMPR 2014.003, with RSDr ranging from 1.4 to 4.7% and RSDR ranging from 8.1 to 11.6%. The adult nutritional sample returned results outside the range of SPMR, having repeatability (RSDr) of 9.9%, higher than the SMPR target of ≤ 6%, and reproducibility (RSDR) of 12.1%, just above the SMPR target of ≤ 12%.
{"title":"Determination of β-Galactooligosaccharides (GOS) in Infant Formula: Collaborative Study, Final Action 2021.01","authors":"Denis Cuany, Sean Austin","doi":"10.1093/jaoacint/qsae031","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae031","url":null,"abstract":"Background We previously published a method for the determination of β-Galactooligosaccharides (GOS) in Infant Formula and Adult Nutritionals which is currently First Action AOAC Method 2021.01. In this study, reproducibility data were collected to support the promotion of the method to Final Action. Method A collaborative study was organized, to which 14 laboratories from eight different countries participated. Initially, laboratories were requested to analyze two practice samples and request guidance from the study director in case of issues. Successful laboratories proceeded to analyze seven samples (six infant formula and one adult nutritional) received as blind duplicates. Results Thirteen laboratories reported acceptable results for practice sample 1. Practice sample 2 could only be delivered to eight of the laboratories due to restrictions at customs. The 13 laboratories successfully analyzing practice sample 1 were requested to continue with the analysis of the MLT samples. Laboratory 14 was unable to solve some technical difficulties, so their data could not be used. Out of the seven samples tested, results for six infant formula met the requirements of the AOAC SMPR 2014.003, with RSDr ranging from 1.4 to 4.7% and RSDR ranging from 8.1 to 11.6%. The adult nutritional sample returned results outside the range of SPMR, having repeatability (RSDr) of 9.9%, higher than the SMPR target of ≤ 6%, and reproducibility (RSDR) of 12.1%, just above the SMPR target of ≤ 12%.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"54 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140578309","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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