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Pages: 529 - 537 Abstract: AbstractBackgroundGalidesivir hydrochloride (GDV) is a new potent and safe antiviral drug used for the treatment of a broad spectrum of viral diseases, including COVID-19. In the literature, no analytical method exists for the determination of GDV in bulk or dosage form.ObjectiveThe objective of this study was the investigation of oxidation reactions of GDV with five inorganic oxidizing reagents and the employment of the reactions in the development of five green microwell spectrophotometric methods (MW-SPMs) with simple procedure and high throughputs for determination of GDV in its bulk and dosage forms (capsules).MethodsThe reactions were carried out in 96-well plates, and the absorbances of reaction solutions were measured by an absorbance microplate reader. Variables influencing the reactions were carefully investigated and optimized.ResultsUnder the refined optimum conditions, Beer’s law with excellent correlation coefficients (0.9992–0.9997) was followed in GDV concentrations in a general range of 5–700 µg/mL, and the limits of detection were ≥1.8 µg/mL. All validation parameters of all methods were acceptable. The methods were successfully applied to the analysis of GDV in bulk drug and capsules with high accuracy and precision; the recovery percentages were 98.6–101.2 ± 0.58–1.14%. The greenness of MW-SPMs was evaluated by three comprehensive metric tools, which demonstrated the adherence of MW-SPMs to the principles of the green analytical chemistry (GAC) approach.ConclusionsThe proposed MW-SPMs combined the advantages of microwell-based practice and the use of common laboratory reagents for the analysis. The advantages of microwell analysis were the high throughput, readily available for semi-automation, reduced samples/reagents volume, precise measurements, and versatility. The advantages of using common laboratory reagents were the availability, consistency, compatibility, safety, and cost-effectiveness.HighlightsOverall, the proposed MW-SPMs are versatile, valuable tools for the quantitation of GDV during its pharmaceutical manufacturing. PubDate: Sat, 23 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae026 Issue No:Vol. 107, No. 4 (2024)
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Pages: 538 - 548 Abstract: AbstractBackgroundTulathromycin (TUL) is a triamilide antibacterial drug which has been approved for use in the European Union and the United States for the treatment and prevention of bovine respiratory diseases. The existing methods for determination of TUL in its pharmaceutical bulk form are very limited and suffer from major drawbacks.ObjectivesThe aim of this study was the development of two innovative microwell spectrophotometric methods (MW-SPMs) for determination of TUL in its pharmaceutical bulk form.MethodsThe formation of charge-transfer complexes (CTCs) of TUL, as an electron donor, was investigated with 2,5-dihydroxy-3,6-dichlorocyclohexa-2,5-diene-1,4-dione (HCD) and 2,3-dichloro-5,6-dicyano-p-benzoquinone (CBQ), as π-electron acceptors. The CTCs were characterized using UV-Vis spectrophotometry and computational calculations. The reactions were employed for the development of two MW-SPMs with one step for the quantitative analysis of TUL.ResultsThe formation of CTCs was confirmed via the formation of characteristic absorption bands with maximum absorption at 520 and 460 nm for CTCs with HCD and CBQ, respectively. The stoichiometry of both CTCs was found to be 1:1, and the values of different spectroscopic and electronic constants confirmed the stability of the CTCs. The mechanisms of the reactions were postulated. The linear range of both MW-SPMs was 10–500 µg/mL. The LOQs were 13.5 and 26.4 µg/mL for methods involving reactions with HCD and CBQ, respectively. Both methods were successfully applied to the quantitation of TUL in pharmaceutical bulk form with acceptable accuracy and precision. The results of eco-friendliness/greenness assessment proved that both MW-SPMs fulfill the requirements of green analytical approaches. In addition, the one-step reactions and simultaneous handling of a large number of samples with micro-volumes in the proposed methods gave them the advantage of high-throughput analysis.ConclusionThis study described two new MW-SPMs as valuable analytical tools for the determination of TUL.HighlightThe proposed methods are valuable analytical tool for the analysis of bulk form of TUL. PubDate: Tue, 23 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae035 Issue No:Vol. 107, No. 4 (2024)
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Pages: 549 - 557 Abstract: AbstractBackgroundThrough 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.ObjectiveFour novel eco-friendly ion selective electrodes (ISE) were generated to determine Ethamsylate (ETM) in bulk powder and different pharmaceutical formulations. The present electrodes were fabricated 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 used for stability-indicating methods.MethodsThe 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 and 2 were fabricated using tetradodecylammonium bromide as an anionic exchanger, adding 4-sulfocalix-8-arene as an ionophore only to electrode 2 and preparing electrode 1 without incorporation of an ionophore. The fabrication of electrodes 3 and 4 was based on ethamsylate–tetraphenylborate (ETM–TPB) as an ion-association complex in a PVC matrix. The environmental sustainability was assessed using the green analytical procedure index (GAPI), and analytical greenness metric for sample preparation (AGREEprep).ResultsElectrodes 1 and 2 had linear dynamic ranges of 10−1–10−5 mol/L and 10−1–10−4 mol/L, respectively, with a Nernstian slope of 49.6 and 53.2 mV/decade, respectively. Electrodes 3 and 4 had linear dynamic ranges of 10−1–10−4 mol/L, with a Nernstian slope of 43.9 and 40.2 mV/decade, respectively.ConclusionThe electrodes' selectivity coefficients showed good selectivity for ETM. The utility of 4-sulfocalix-8-arene as an ionophore had a significant influence on increasing the membrane sensitivity and selectivity of electrode 2 compared to other electrodes.HighlightsFour novel eco-friendly ISEs were used for determination of ETM in bulk powder and different pharmaceutical formulations. Different experimental parameters were performed to optimize the determination conditions such as solvent mediators, dynamic response time, effect of pH, and temperature. Stability-indicating measurement of ETM in the presence of its degradate HQ and co-formulated drug tranexamic acid. Using new ecological assessment tools to determine whiteness and greenness profiles. PubDate: Tue, 16 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae034 Issue No:Vol. 107, No. 4 (2024)
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Pages: 558 - 570 Abstract: AbstractBackgroundEstimation of the drug and development of the method is a critical aspect of formulation development and a critical factor for analytical scientists. Gefitinib is a poorly soluble anticancer drug.ObjectiveThe present research focuses on the topic of the development of innovative quality by design methods for the estimation of gefitinib (GF) from bulk, pharmaceutical tablet formulation, and complex nanoformulations.MethodsTo simplify the estimation of poorly soluble drugs such as GF, response surface methodology (RSM) was adopted with effective leverages to obtain precise computation design space using the Box-Behnken design (BBD) model. The major three mixed-effect independent factors (percentage of buffer, pH of buffer, and flow rate) were screened with three prominent dependent responses (viz., theoretical plate, retention time, and tailing factor) selected for optimal analysis. Furthermore, co-processed steps were employed for the estimation of the analyte from the complex formulation.ResultsThe RP-HPLC method uses the quality by design (QbD) approach can effectively estimate the analyte concentration of less than 4.5 min. The developed method was economically robust and sensitive and shows a relative standard deviation (RSD, %) of less than 2% for all the selected validation parameters. The estimated design space suggests the highest desirability (R2—0.998) at 60% of buffer in the mobile phase, pH 4.25, and flow rate of 0.7 mL/min.ConclusionsThe QbD approach was used to design and develop the method by understanding the interaction between dependent and independent variables to get the optimum values. The developed method was validated successfully and can be useful for formulation scientists to estimate drug concentration and drug release profiles from complex nanoformulations.HighlightsThe analytical approach was designed and quantified using a quality-by-design approach to make the RP-HPLC method more robust and efficient for the estimation of analytes from complex nanoformulations. The method is also useful to eliminate the interfering molecule during estimation by employing co-processing steps. The developed method saves time and cost of solvent and employs QbD as a requirement of recent regulatory concern. PubDate: Mon, 22 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae033 Issue No:Vol. 107, No. 4 (2024)
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Pages: 571 - 581 Abstract: AbstractBackgroundThe topical veterinary drug product containing fipronil and permethrin provides an effective repellent protection and high insecticidal efficacy for dogs.ObjectiveThe objective of this study was to develop a stability-indicating high-performance liquid chromatography (HPLC) method for simultaneous detection and quantification of fipronil, permethrin, their key degradation products, and butylated hydroxytoluene (BHT) in a topical drug product.MethodThe two active ingredients, their degradation products, and the antioxidant (BHT) were separated by a gradient elution on a Phenomenex Kinetex C18 column (150 × 3 mm, 2.6 µm particle size) maintained at 37°C with H2O “acetonitrile “isopropyl alcohol “85% H3PO4 (65.5 + 32.5 + 4/0.0053, v/v/v/v) as mobile phase A and acetonitrile (100%) as mobile phase B. The flow rate was 0.9 mL/min, and analytes were detected and quantified at 235 nm.ResultsThe specificity of the method was demonstrated by adequate separation of fipronil, permethrin, their degradation products, and BHT in the forced degraded finished product. The linearity of the method was demonstrated in the range of 0.2% to 150% of target analytical concentration of both active ingredients and 50% to 150% for BHT. Excellent recoveries of fipronil, permethrin, and BHT in placebo spiked active ingredient solutions in the linearity range showed sufficient accuracy of the method. The LOQ and LOD of the method were determined to be 0.2% and 0.07% of the analytical concentration. A robustness study did not identify any critical parameter that adversely affected the separation and quantification.ConclusionsHere, we report the development and validation of a robust, stability-indicating HPLC method for identification and assay of fipronil, permethrin, and BHT, including estimation of fipronil’s and permethrin’s degradation products in a topical drug product for dogs.HighlightsThe new HPLC method permits the acquisition of data for all analytes of interest for a topical finished drug product containing fipronil, permethrin, and BHT. PubDate: Thu, 25 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae037 Issue No:Vol. 107, No. 4 (2024)
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Pages: 582 - 591 Abstract: AbstractBackgroundBusulfan is the most effective medication for treating chronic myelogenous or granulocytic leukemia because it has cytotoxic properties that harm or kill hematopoietic cells. It cannot absorb light in the Ultraviolet range due to its structure. Because of this, it is very challenging to quantify using traditional HPLC coupled with UV/Photodiode Array detectors. So, using sodium diethyldithiocarbamate, a derivatization method was developed to quantify related impurities. A significant unknown impurity was identified in derivatized samples of busulfan and a noticeably high percentage level was discovered during routine drug testing.ObjectiveWe aimed to isolate, and characterize the unknown impurity observed in the samples and to identify its root cause.MethodsPreparative HPLC was used to isolate the unidentified, derivatized impurity, and 1H NMR, 13C NMR, and MS were used to decipher its structural components.ResultsThe spectral characterization data analysis showed that the unknown impurity was related to busulfan. Additionally, it was noted that the impurity developed as a result of the residual buffer used to prepare the derivatizing reagent.ConclusionThe isolated impurity was found to be same as comparable to that found in busulfan drug substances, according to the results of the characterization tools. An alternative method of reagent preparation was optimized and deemed satisfactory because the buffer used in reagent preparation is the only factor contributing to the formation of impurities.HighlightsUsing cutting-edge analytical characterization tools, it was possible to explain the structural characteristics of an unknown impurity and discover that it was a novel impurity, which undoubtedly contributes to the comprehension of drug substance reaction properties. PubDate: Sat, 02 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae018 Issue No:Vol. 107, No. 4 (2024)
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Pages: 592 - 599 Abstract: AbstractBackgroundTo study the ultra-trace simultaneous determination of drugs, the colorimetric method in combination with chemometrics can be used.ObjectiveIn this study, a simple, rapid, and sensitive UV-Vis spectrophotometric method using gold nanoparticles (AuNPs) was introduced for the simultaneous determination of ultra-trace amounts of pilocarpine (PIL) and timolol (TIM) in binary mixtures and biological samples.MethodsAuNPs interacted with components and the aggregation mode of NPs occurred, and, finally, the color change of the solution (red to gray) was observed with the naked eye without the most modern and expensive instruments. The characterization of AuNPs was evaluated by transmission electron microscopy (TEM) and dynamic light scattering (DLS).ResultsThe validation of the colorimetric way was studied in the concentration range of 100–800 and 100–600 μg/L with good linearity equal to 0.9772 and 0.9891 for PIL and TIM, respectively. The limit of detection (LOD) was found to be 165.00 and 92.40 μg/L, where the limit of quantitation (LOQ) was 500.00 and 280.00 μg/L for PIL and TIM, respectively. The effect of some factors such as interaction time, the concentration of components, and the volume of buffer on absorbance was investigated. Partial least squares (PLS) as an efficient multivariate calibration method was combined with colorimetry for the simultaneous determination of PIL and TIM in binary mixtures. The optimum number of latent variables was selected by k-fold cross-validation based on minimum mean square error prediction (MSEP), and the number of components equal to 1 with MSEP of 1.085 and 0.763 was considered for PIL and TIM, respectively. The mean recovery was obtained at 100.20 and 101.55% for PIL and TIM, respectively.ConclusionsThe colorimetric method can be introduced as a proper option for the simultaneous determination of components in pharmaceutical formulations and other samples.HighlightsA colorimetric method using AuNPs was proposed. The PLS method was coupled with a colorimetric method for the ultra-trace simultaneous estimation of PIL and TIM in binary mixtures. Ultra-trace amounts of PIL and TIM were also determined in biological samples. The proposed method is simple, fast, and less expensive than chromatography methods. PubDate: Fri, 12 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae030 Issue No:Vol. 107, No. 4 (2024)
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Pages: 600 - 607 Abstract: AbstractBackgroundFipronil is a commonly used pesticide in the agricultural and animal health industries for the protection of crops and control of fleas, ticks, and chewing lice. It is difficult to obtain reproducible retention time and relative retention time (RRT) for a common hydrolytic degradation product of fipronil with the current European Pharmacopeia (EP) monograph for assay and estimation of related substances of fipronil. This situation causes misidentification, mislabeling, and/or false out-of-specification results for this hydrolytic degradation product of fipronil in bulk commercial batches during batch release and/or in the stability samples during the shelf life of a released batch.ObjectiveThis study aimed to develop a reversed-phase ultra performance liquid chromatography (UPLC) method for assay and identification of fipronil including identification and estimation of its related substances in bulk drug substance batches of fipronil and provide consistent retention time of the hydrolytic degradation product.MethodsFipronil and its related substances were separated by gradient elution on a Halo C18 column (50 mm × 2.1 mm id, 2.0 µm particle size) maintained at 40°C with 0.1% H3PO4 in H2O as mobile phase-A and acetonitrile–methanol (50 + 50, v/v) as mobile phase-B. Fipronil and its related substances were detected and quantified at 280 nm with a quantitation limit of 0.05% of the target (analytical) concentration.ResultsThe UPLC method was able to separate all analytes of interest by gradient elution with a total run time of 7 min (approximately 40% faster than EP).ConclusionIn this paper, we report the development and validation of a fast, stability-indicating reversed-phase UPLC method for assay and estimation of related substances of fipronil in stability samples and bulk batches of fipronil.HighlightsThe new UPLC method is approximately 40% faster than the current Ph. Eur. monograph for fipronil assay and the new method provides reproducible retention of a common hydrolytic degradation product of fipronil. PubDate: Tue, 26 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae027 Issue No:Vol. 107, No. 4 (2024)
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Pages: 608 - 616 Abstract: AbstractBackgroundDetermining the concentration of nanoparticles (NPs) in marine organisms is important for evaluating their environmental impact and to assess potential food safety risks to human health.ObjectiveThe current work aimed at developing an in-house method based on single-particle inductively coupled plasma-mass spectrometry (SP-ICP-MS) suitable for surveillance of NPs in mussels.MethodsA new low-cost and simple protease mixture was utilized for sample digestion, and novel open-source data processing was used, establishing detection limits on a statistical basis using false-positive and false-negative probabilities. The method was validated for 30 and 60 nm gold NPs spiked to mussels as a proxy for seafood.ResultsRecoveries were 76–77% for particle mass concentration and 94–101% for particle number concentration. Intermediate precision was 8–9% for particle mass concentration and 7–8% for particle number concentration. The detection limit for size was 18 nm, for concentration 1.7 ng/g, and 4.2 × 105 particles/g mussel tissue.ConclusionThe performance characteristics of the method were satisfactory compared with numeric Codex criteria. Further, the method was applied to titanium-, chromium- and copper-based particles in mussels.HighlightsThe method demonstrates a new practical and cost-effective sample treatment, and streamlined, transparent, and reproducible data treatment for the routine surveillance of NPs in mussels. PubDate: Wed, 20 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae024 Issue No:Vol. 107, No. 4 (2024)
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Pages: 617 - 631 Abstract: AbstractBackgroundThe 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 INTERNATIONAL identified the need for a reliable confirmatory screening method. Such a qualitative approach is required for compliance checking and to support product release in manufacturing.ObjectiveData were collected from five independent laboratories that applied the First Action Official Method 2020.04 to demonstrate adequate performance under reproducibility conditions. The 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 evaluated by participating in 92 proficiency tests.MethodsFour 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 based on 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).ResultsThe multilaboratory validation led to PODs at the STC ≥94% and PODs in the blank ≤9%. Further application of the multilaboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784).ConclusionThe interlaboratory reproducibility determined for this method met the acceptance criteria defined in AOAC Standard Method Performance Requirement (SMPR®) 2018.010.HighlightsAOAC has approved the method for Final Action status. PubDate: Tue, 16 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae032 Issue No:Vol. 107, No. 4 (2024)
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Pages: 632 - 640 Abstract: AbstractBackgroundAn interlaboratory study was conducted at the U.S. Food and Drug Administration’s (FDA) Northeast Food and Feed Laboratory (NFFL) and the Center for Food Safety and Applied Nutrition (CFSAN) with the purpose to expand FDA Elemental Analysis Manual (EAM) method 4.7 (Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion) to include new analytes.ObjectiveThe goal of the study was to demonstrate the performance of FDA EAM method 4.7 when analyzing new analytes cobalt (Co), strontium (Sr), thallium (Tl), tin (Sn), uranium (U), and vanadium (V). This analyte extension method validation of EAM 4.7 for six additional elements, Co, Sr, Tl, Sn, U, and V, followed all guidelines for a Level 2 or single-laboratory validation and met all acceptance criteria for analyte extensions as per the Guidelines for the Validation of Chemical Methods.MethodAs per EAM 4.7, this study followed the procedures and used specified equipment operated under recommended conditions. The analyte extension method validation was performed in accordance with protocol and with no deviations.ResultsAll quality control (QC) requirements for this analyte extension method validation of EAM 4.7 passed as evidenced by the analytical data. The results presented demonstrate accuracy, linearity, and precision by successful analyses of method blanks, matrix spikes, unfortified test samples, and reference materials. The data analyzed met each of the validation requirements for each analyte in all representative matrixes.ConclusionsThe study showed that the new analytes performed satisfactorily using EAM 4.7 for total acidic extractable elemental analysis of food according to FDA’s guidelines.HighlightsThe method met or exceeded the performance criteria. PubDate: Tue, 02 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae029 Issue No:Vol. 107, No. 4 (2024)
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Pages: 641 - 648 Abstract: AbstractBackgroundTo protect public and animal health against risks provoked by aflatoxins contained therein, maximum limits for aflatoxins are defined. Limit values vary depending on the intended use and regulatory authority, therefore quantitative detection is essential.ObjectiveValidation of a one-step competitive lateral flow immunochromatographic assay for quantitative screening of total aflatoxin (B1, B2, G1, and G2) in corn and peanut paste for the high-sensitivity range (0–50 µg/kg).MethodsCorn or peanut paste test portions are water-based extracted and prepared for testing within 15 min. The AgraStrip® Pro Total Aflatoxin WATEX® test method quantifies the concentration of aflatoxins in the sample. Selectivity, robustness, product consistency, and stability testing were performed in addition to matrix testing.ResultsNo cross-reactivity was detected against possible interferants. Corn resulted in a LOD and LOQ of 0.9 and 2.8 µg/kg and overall recoveries between 74 and 108%. Peanut paste resulted internally in a LOD and LOQ of 0.8 and 2.3 µg/kg and recoveries between 86 and 98%. Stability testing showed no influence of the age of the respective lot on the result. Robustness testing demonstrated that varying the amount of water used for extraction, extraction time, and delay between extract dilution and analysis did not significantly affect the result. Due to supply chain issues, a change to the outer cartridge required an increase in the test aliquot size, which had no effect on method performance.ConclusionThe test kit was validated for the determination of total aflatoxins in corn and peanut paste. Recovery and precision met the requirements laid down in Codex Alimentarius CXG 71–2009 and acceptable robustness, selectivity, and product consistency and stability were demonstrated.HighlightsThe AgraStrip Pro Total Aflatoxin WATEX test kit in the high sensitivity range (0–50 µg/kg) was approved by the AOAC AOAC Research Institute (PTM number 032402). PubDate: Mon, 13 May 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae040 Issue No:Vol. 107, No. 4 (2024)
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Pages: 649 - 662 Abstract: AbstractBackgroundAntibiotic residues in milk are a well-known hazard in the dairy food chain. Detection methods for these residues, such as nonspecific microbiological inhibitor tests or group-specific receptor tests, are relatively inexpensive, easy to use, and widely applied to ensure food safety. In contrast, specific detection by liquid chromatography–tandem mass spectrometry (LC–MS/MS)—although a critical, complimentary method to confirm the results of nonspecific testing—is relatively costly, time-consuming, and laborious. Furthermore, sample processing before LC–MS/MS analysis requires unique preparation procedures for different groups of antibiotic compounds.ObjectiveTo simplify and speed up specific antibiotic residue detection, a low-cost, passive, and single-step method to fractionate analytes in raw milk was developed.MethodsUntreated raw milk was fractionated into its water and fat/protein phases using a Fractionation of Milk for Trace Analysis of Contaminants and Residues for Antibiotics (FraMiTrACR® AB) fractionation unit. The water fraction was then analyzed by LC–MS/MS. The analyte fractionation method was evaluated against a Quick Easy Cheap Effective Rugged and Safe (QuEChERS)-based method for sample preparation.ResultsOur method allows qualitative and quantitative detection of substances from the penicillin, cephalosporin, macrolide, lincosamide, sulfonamide, tetracycline, and fluoroquinolone groups of antibiotics. Detection limits are below the legally prescribed maximum residue levels, allowing reliable, specific, and rapid validation of a positive result in nonspecific microbiological inhibitor tests.ConclusionAnalyte fractionation by FraMiTrACR AB is a faster alternative to QuEChERS-based sample preparation for the detection of antibiotic substances in milk.HighlightThis method describes a low-cost, environmentally friendly, passive, and single-step milk analyte fractionation. As an alternative to QuEChERS-based preparation, this fractionation method simplifies and speeds up the process for specific antibiotic residue detection. PubDate: Mon, 11 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae022 Issue No:Vol. 107, No. 4 (2024)
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Pages: 663 - 678 Abstract: AbstractBackgroundDietary supplements derived from botanicals are commonly consumed and investigated in biomedical studies for their potential health benefits. Accurate identification and quantification of key chemical constituents from botanical ingredients is necessary for consistent product preparations and reproducible research results. Manufacturers need quantitative reference materials of the chemical constituents of interest to verify the content of ingredients and products. The rigor and reproducibility of biomedical research is enhanced through thorough characterization of the interventions used in mechanistic, clinical, and safety investigations. Quantitative reference materials enable reliable product quality assessments and reproducible research results.ObjectiveSolution-based certified reference material (CRM) mixes were developed as calibrants for phytochemicals in ginger and kava. The kava CRM contained yangonin, desmethoxyyangonin, dihydrokavain, DL-kavain, methysticin, dihydromethysticin, flavokawain A, flavokawain B, and flavokawain C. The ginger CRM contained 6-gingerol, 8-gingerol, 10-gingerol, 6-shogaol, 8-shogaol, and 10-shogaol.MethodsEach phytochemical was sourced as an isolated compound and assigned a purity factor by a mass balance approach accounting for residual impurities. The solution standard mixes were formulated by gravimetric addition of each phytochemical incorporating the purity factor and diluting with acetonitrile to the target concentrations of 500 µg/mL for the gingerols and shogaols, 250 µg/mL for the kavalactones, and 25 µg/mL for the flavokawains.ResultsThe concentration accuracy of each component in the solution mixes was analytically verified by ultra high performance liquid chromatography with ultraviolet detection (UHPLC–UV) assay comparison to an independently prepared calibration solution. Each component in the ginger and kava CRMs were within 5 and 7% of the target concentrations, respectively.ConclusionHomogeneous kava and ginger phytochemical solution mixes were produced with accurate constituent concentrations and demonstrated good stability over 2 years. These solution mixes were launched as commercially available CRMs.HighlightsThese mixes can be used as accurate concentration stock solutions to prepare calibrators and controls for botanical dietary supplement product testing and standardization. PubDate: Tue, 26 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae025 Issue No:Vol. 107, No. 4 (2024)
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Pages: 679 - 692 Abstract: AbstractBackgroundWe 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.MethodsA collaborative study was organized in 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.ResultsThirteen 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 multilaboratory trial (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 formulas met the requirements of the AOAC Standard Method Performance Requirements (SMPR®) 2014.003, with repeatability (RSDr) ranging from 1.4 to 4.7% and reproducibility (RSDR) ranging from 8.1 to 11.6%. The adult nutritional sample returned results outside the range of the SMPR, having an RSDr of 9.9%, higher than the SMPR target of ≤6%, and an RSDR of 12.1%, just above the SMPR target of ≤12%.ConclusionThe method described is suitable for the determination of GOS in infant formula.HighlightA method is described which is suitable for the determination of GOS in infant formula. PubDate: Sat, 13 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae031 Issue No:Vol. 107, No. 4 (2024)
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Pages: 693 - 704 Abstract: AbstractBackgroundInfant formulas, and pediatric and adult nutritional products, are being fortified with bovine lactoferrin (bLF) due to its beneficial impacts on immune development and gut health. Lactoferrin supplementation into these products requires an analytical method to accurately quantify the concentrations of bLF to meet global regulatory and quality standards.ObjectiveTo develop and validate a lactoferrin method capable of meeting the AOAC INTERNATIONAL Standard Method Performance Requirements (SMPR®) 2020.005.MethodsPowder formula samples are extracted using warm dibasic phosphate buffer, pH 8, then centrifuged at 4°C to remove insoluble proteins, fat, and other solids. The soluble fraction is further purified on a HiTrap heparin solid-phase extraction (SPE) column to isolate bLF from interferences. Samples are filtered, then analyzed by LC–UV using a protein BEH C4 analytical column and quantitated using an external calibrant.ResultsThe LOQ (2 mg/100 g), repeatability (RSD: 2.0–4.8%), recovery (92.1–97.7%), and analytical range (4–193 mg/100 g) all meet the method requirements as stated in SMPR 2020.005 for lactoferrin.ConclusionThe reported single-laboratory validation (SLV) results demonstrate the ability of this lactoferrin method to meet or exceed the method performance requirements to measure soluble, intact, non-denatured bLF in infant and adult nutritional powder formulas.HighlightsThe use of a heparin affinity column to isolate lactoferrin from bovine milk products combined with a selective analytical chromatographic column provides suitable analyte specificity without requiring proprietary equipment or reagents. PubDate: Sat, 04 May 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae038 Issue No:Vol. 107, No. 4 (2024)
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Pages: 704 - 713 Abstract: AbstractBackgroundArcae concha and Meretricis concha cyclinae concha are two marine shellfish herbs with similar composition and efficacy, which are usually calcined and used clinically.ObjectiveThis study investigated variations in the inorganic and organic components of Arcae concha and Meretricis concha cyclinae concha from different production regions, both Arcae concha and Meretricis concha cyclinae concha. The aim was to enhance the understanding of these two types of marine shell traditional Chinese medicine (msTCM) and provide a foundation for their future development and application.MethodSpectroscopic techniques, including infrared spectroscopy, X-ray spectroscopy, and X-ray fluorescence spectroscopy, were used to analyze the calcium carbonate (CaCO3) crystal and trace elements. Thermogravimetric analysis was used to investigate the decomposition process during heating. The proteins were quantified using the BCA protein assay kit. Principal component analysis (PCA) was used to classify inorganic elements in the two marine shellfish traditional Chinese medicines.ResultsNo significant differences were found among the various production regions. The crystal structure of CaCO3 in the raw products was aragonite, but it transformed into calcite after calcination. The contents of Ca, Na, Sr, and other inorganic elements were highest. The protein content was significantly reduced after calcination. Therefore, these factors cannot accurately reflect the internal quality of TCM, rendering qualitative identification challenging. CaCO3 dissolution in the decoction of Arcae concha and Meretricis concha cyclinae concha increased after calcination, aligning with the clinical application of calcined shell TCM. PCA revealed the inorganic elements in them, indicating that the variation in trace element composition among different drugs leads to differences in their therapeutic focus, which should be considered during usage.ConclusionsThis study clarifies the composition and structure changes of corrugated and clam shell before and after calcining, and it lays the foundation for the comprehensive utilization of marine traditional Chinese medicine.HighlightsThese technical representations reveal the differences between raw materials and processed products, which will provide support for the quality control of other shellfish TCM. PubDate: Sat, 16 Mar 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae023 Issue No:Vol. 107, No. 4 (2024)
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Pages: 714 - 726 Abstract: AbstractBackgroundCassia (Family: Fabaceae) species are a large group of flowering plants rich in bioactive anthraquinone and flavonoids used in botanical supplements and nutraceuticals.ObjectiveA simple and reliable high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and validated for separating and quantifying 13 anthraquinone and flavonoids. These compounds were further confirmed using an LC-based electrospray ionization mass spectrometry (ESI-MS/MS) method in the leaves and flowers of selected Cassia species. A simple and rapid HPTLC method was developed for chemical fingerprint analysis of all Cassia species.MethodAll 13 compounds were chromatographically separated on a Zorbax TC18 (4.6 × 250, 5 μm particle size) analytical column, and 0.1% formic acid and acetonitrile as elution solvents at a flow rate of 0.8 mL/min with detection at 259 nm. For HPTLC fingerprinting, the mobile phase compositions of toluene, ethyl acetate, and formic acid (5.5:4.2:0.6, v/v/v) were optimized to separate and identify all compounds using silica gel 60F254 aluminum plates.ResultsThe validation data for the developed HPLC-PDA method for 13 compounds showed good linearity (r2 >0.99) with a sensitive LOD (0.082–1.969 μg/mL), LOQ (0.250–5.967 μg/mL), and excellent recoveries (85.22–100.32%). The quantification results were found to be precise and accurate (<5.0% and relative error), -0.77–0.44 with ESI-MS/MS confirmation in the Cassia samples. The novel HPTLC method was excellent separation for 13 compounds, with Rf values ranging between 0.12 and 0.61.ConclusionsThe developed HPLC-PDA method was simple and precise and could separate and quantify anthraquinones and flavonoids along with confirmation, using a novel LC-based ESI-MS/MS. The HPTLC method was found to be simple and precise, with excellent separation capabilities for these compounds.HighlightsThis novel multiplatform approach successfully identified and quantified 13 compounds simultaneously using an integration of data strategy in seven medicinally important Cassia species’ leaves and flowers. PubDate: Mon, 22 Apr 2024 00:00:00 GMT DOI: 10.1093/jaoacint/qsae028 Issue No:Vol. 107, No. 4 (2024)
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