Journal of AOAC International

BACKGROUND: Tulathromycin (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. OBJECTIVES: The aim of this study was the development of two innovative microwell spectrophotometric methods (MW-SPMs) for determination of TUL in its pharmaceutical bulk form...

BACKGROUND: Cassia (Family: Fabaceae) species are a large group of flowering plants rich in bioactive anthraquinone and flavonoids used in botanical supplements and nutraceuticals. OBJECTIVE: A simple and reliable high-performance liquid chromatography-photodiode array (HPLC-PDA) method was developed and validated for separating and quantifying thirteen 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...

BACKGROUND: Estimation 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. OBJECTIVE: The present research enlightens 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. METHODS: To simplify the estimation of poorly soluble drugs like GF, Response Surface Methodology (RSM) was adopted with effective leverages to obtain precise computation design space using the Box-Behnken Design (BBD) model...

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...

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...

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...

BACKGROUND: To study the ultra-trace simultaneous determination of drugs, the colorimetric method in combination with chemometrics can be used. OBJECTIVE: In 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 sample. METHODS: AuNPs 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...

BACKGROUND: An 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 (1). OBJECTIVE: The goal of the study was to demonstrate the performance of FDA EAM method 4...

BACKGROUND: Fipronil 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 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-specifications 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...

BACKGROUND: Dietary 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...

BACKGROUND: Galidesivir 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 and dosage form. OBJECTIVE: The 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)...

BACKGROUND: Determining the concentration of nanoparticles in marine organisms is important for evaluating their environmental impact and to assess potential food safety risks to human health. OBJECTIVE: The current work aimed at developing an in-house method based on single particle inductively coupled plasma mass spectrometry suitable for surveillance of nanoparticles in mussels. METHOD: A new low-cost and simple protease mixture was utilized for sample digestion, and a novel open-source data processing was used, establishing detection limits on a statistical basis using false positive and false negative probabilities...

BACKGROUND: Arcae concha and Meretricis concha cyclinae concha are two marine shellfish herbs with similar composition and efficacy, which are usually calcined and used clinically. OBJECTIVE: This 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...

BACKGROUND: The use of stable carbon isotope ratios (δ13C) of sugar fractions of honey is a powerful tool to detect adulteration with sugar syrups. This is accomplished by calculating differences of the δ13C values between individual honey saccharides and comparing them to published purity criteria. A liquid chromatography-isotope ratio mass spectrometry (LC-IRMS) method for the determination of δ13C values of sugars in honey was previously validated by an interlaboratory comparison but no further guidance was given how to include the obtained precision figures of the compound specific δ13C values in the purity assessment of honey...

BACKGROUND: Antibiotic residues in milk are a well-known hazard in the dairy food chain. Detection methods for these residues, such as non-specific microbiological inhibitor tests or group-specific receptor tests, respectively, 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 non-specific testing-is relatively costly, time consuming and laborious...

BACKGROUND: Ponceau 4R (E124) and Carmoisine (E122) are frequently utilized azo synthetic dye in the food industry owing to their aesthetically pleasing coloration and broad consumer acceptability. It is imperative to prioritize environmentally favorable technologies for quantifying these dyes, as excessive consumption of those poses significant health risks. OBJECTIVE: The primary objective of this research was to establish a Reversed Phase High Performance Liquid Chromatography (RP-HPLC) method that could simultaneously detect Ponceau 4R and Carmoisine, implementing green analytical chemistry (GAC) and analytical quality by design (AQbD) employing ultrasound-assisted extraction (UAE) technique in commercial food samples...

BACKGROUND: Busulfan 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/PDA 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 with a noticeably high percentage level was discovered during routine drug testing...

BACKGROUND: Food allergen cross-contact during food preparation and production is one of the causes of unintentional allergen presence in packaged foods. However, little is known about allergen cross-contact in shared frying or roasting oil, which prevents the establishment of effective allergen controls and may put allergic individuals at risk. To better understand the quantity of allergen transferred to frying oil and subsequent products, an analytical method is needed for quantifying protein in oil that has been exposed to frying/roasting conditions...

BACKGROUND: The leaves of Elaeagnus angustifolia, belonging to the Elaeagnaceae Juss. family, are known for their medicinal properties for relieving cough and asthma, as well as treating dysentery and diarrhea. OBJECTIVE: To establish a rapid qualitative method for the detection of secondary metabolites in leaves of Elaeagnus angustifolia, including the identification and analysis of various secondary metabolites in leaves of Elaeagnus angustifolia. METHOD: Samples were separated using a Waters ACQUITY H-Class ultra-performance liquid chromatography (UPLC) system (FTN autosampler, quaternary LC pump) and ACQUITY UPLC® BEH C18 column (1...

While current analytical methodologies can readily identify cannabis use, definitively establishing recent use within the impairment window has proven to be far more complex, requiring a new approach. Recent studies have shown no direct relationship between impairment and Δ9-tetra-hydrocannabinol (Δ9-THC) concentrations in blood or saliva, making legal "per se" Δ9-THC limits scientifically unjustified. Current methods that focus on Δ9-THC and/or metabolite concentrations in blood, saliva, urine, or exhaled breath can lead to false positive results for recent use due to the persistence of Δ9-THC well outside of the typical three to four-hour window of potential impairment following cannabis inhalation...