Journal of AOAC International最新文献

Background: Botanical reference materials (BRMs) generally account for the species, cultivar, and year and location of harvest that result in variability in the chemical composition that may lead to statistically significant differences using chemometric methods.

Objective: To compare the chemical composition of five species of Actaea root BRMs, four herbal sources of A. racemosa root BRMs, and A. racemosa BRMS, and commercial roots and supplements using chemometric methods and selected pre-processing approaches.

Method: Samples were analyzed by flow injection mass spectrometry (FIMS), principal component analysis (PCA), and factorial multivariate analysis of variance (mANOVA).

Results: Statistically significant (P = 0.05) compositional differences were found between three genera (Actaea, Panax, and Ginkgo), five species of Actaea (A. racemosa, A. cimicifuga, A. dahurica, A. pachypoda, and A. rubra) root BRMs, four herbal sources of A. racemosa root BRMs, and A. racemosa BRMS and commercial roots and supplements. The variability of 6% of the BRM variables was found to be quantitatively conserved and reduced the compositional differences between the four sources of root BRMs. Compositional overlap of A. racemosa and other Actaea BRMs was influenced by variation in technical repeats, pre-processing methods, selection of variables, and selection of confidence limits. Sensitivity ranged from 94 to 97% and specificity ranged from 21 to 89% for the pre-processing protocols tested.

Conclusions: Environmental, genetic, and chemometric factors can influence discrimination between species and authentic botanical reference materials.

Highlights: Frequency distribution plots derived from soft independent modeling of class analogy provide excellent means for understanding the impact of experimental factors.

Background: The LactoSens®R method was previously shown to have acceptable accuracy and repeatability precision as required by AOAC Standard Method Performance Requirements (SMPR®) 2018.009 for determination of lactose in low-lactose or lactose-free milk, milk products, and products containing dairy ingredients and was awarded Official Method of AnalysisSM (OMA) First Action status in 2020.

Objective: The method was subjected to a multilaboratory validation (MLV) study to evaluate the reproducibility precision of the method.

Methods: Fourteen validation materials were provided to 15 laboratories in seven countries as blind duplicates. The materials ranged from 0 to 173 mg/100 g lactose. Each laboratory analyzed the blind duplicates according to OMA 2020.01. The data were analyzed for repeatability and reproducibility precision.

Results: RSDr values varied from 2.81 to 8.76%, and RSDR values varied from 4.25 to 12.5%. When sorted by category and concentration range, these results met the repeatability and reproducibility criteria required by SMPR 2018.009.

Conclusions: The data generated in the MLV support the adoption of OMA 2020.01 as Final Action status.

Highlights: The LactoSensR method, as described by OMA 2020.01, provides an accurate and precise determination of lactose in a variety of low-lactose and lactose-free milk, milk products, and products containing dairy ingredients in minutes.

Background: The consumption of foods containing amphenicols, a type of antibiotic, is a major concern for human health. A stable and accurate detection method can provide technical support for food-safety monitoring.

Objective: An effective and efficient method was established for determining amphenicols in animal-derived foods through the simultaneous use of solid-phase extraction (SPE) cleanup and ultrahigh-performance liquid chromatography/mass spectrometry (UPLC-MS/MS).

Method: Samples were extracted using 1.0% ammoniated ethyl acetate solution, degreased with n-hexane, and then concentrated and cleaned using a C18 SPE column. Next, gradient elution was performed using methanol and 0.05% aqueous ammonia as the mobile phase, followed by separation using a C18 column. The target compound was detected using electrospray ionization, both in positive and negative modes, through multiple reaction monitoring, and quantified using an internal-standard method.

Results: The content of chloramphenicol (CAP), florfenicol (FF), and florfenicol amine (FFA) (content range: 0.2-8.0 µg/kg) as well as that of thiamphenicol (TAP; content range: 1.0-40.0 µg/kg) show a good linear relationship, with a correlation coefficient of r > 0.999. Furthermore, recoveries of 86.7-111.9% and relative standard deviations of <9.0% were achieved. The limits of detection and quantification are obtained as 0.03-0.33 and 0.1-1.0 μg/kg, respectively.

Conclusions: The proposed method has excellent stability and accuracy, and can be successfully used for the qualitative and quantitative determination of amphenicols, i.e., CAP, TAP, FF, and FFA residues in 210 animal-derived food samples, of which FF and FFA were detected in four samples.

Highlights: A stable and accurate method was successfully established for the simultaneous determination of CAP, TAP, FF, and FFA in animal-derived foods using UPLC-MS/MS. Effective sample pretreatment was established, lipids were removed using n-hexane, concentration and cleanup were achieved with the C18 SPE column, and matrix effects were effectively reduced, thus improving the method's accuracy and stability. The method was validated for eight common animal-source foods, including beef, lamb, pork, chicken, egg, milk, fish, and honey. This method has good applicability for CAP, TAP, FF, and FFA in animal-derived foods.

Background: A method for sugar profile analysis granted First Action 2018.16 was subjected to a multi-laboratory study.

Objective: Perform a multi-laboratory study with this method to determine the performance parameters of repeatability and reproducibility against the AOAC Standard Method Performance Requirements (AOAC SMPR 2018.001) for Final Action status.

Methods: Eleven laboratories from three different countries participated in the study. Each laboratory was provided practice materials for successful method setup. Each laboratory then proceeded with analysis of blind duplicates of 10 different products covering the scope of the method. Results were reported to the study directors with any modifications and assessed following the procedures of Appendix D of the AOAC Official Methods of AnalysisSM (guidelines for collaborative study procedures).

Results: The majority of results from the study met the SMPR requirements. The data is presented along with any outlying observations or modifications. The method was proven to be flexible across different instrumentation and laboratories, and the method was updated to provide further system suitability and guidelines to maintain the performance of the method across the large scope of matrixes.

Conclusion: The results from the collaborative study supported the method for Final Action status. The Expert Review Panel reviewed and voted to move the method forward to Final Action and was followed by review from the Official Methods Board and granted approval.

Highlights: The method was granted Final Action Official Methods status.

Background: Analytical tests were conducted to investigate the use of N-bromosuccinimide (NBS) as an important, safe analytical reagent for the spectrophotometric detection of therapeutically significant dihydropyridine-based calcium antagonists (DHP), namely nifedipine (NIF) and amlodipine (AML), which have been demonstrated to possess antioxidant activity in vivo and to reduce the intracellular production of reactive oxygen species (ROS). Following the reaction of DHP and NBS in acidic media, the excess NBS was evaluated for the first time by its interaction with P-aminophenol (PAP), which produced a violet-colored product that was detected at 556 nm.

Objective: The analytical method was performed and validated since different variables disturbing the reaction (concentration of reagent, type and concentration of the selected acid, reaction time and the diluting solvents) were carefully studied and optimized.

Methods: The stoichiometry of the applied reaction was determined by Job's method of continuous variation. Monitoring of these drug dosage forms' content uniformity is a first tool or evidence for their efficacy and safety after their administration.

Results: Beer's law was obeyed in the concentration range 1.25-11.0 µg/mL for NIF and 1.25-10.0 µg/mL for AML. The calculated limit of detection (LODs) and limit of quantification (LOQs) for NIF and AML were 0.220, 0.155 µg/mL and 0.519, 0.735 µg/mL, respectively. The precision of the applied method was satisfactory; the RSDs did not exceed 2%. Two greenness assessment tools, the Green Analytical Procedure Index (GAPI) and Analytical Greenness Metric for Sample Preparation (AGREEprep) were used for measuring the environmental friendliness of the recommended method.

Conclusion: The micro-determinations of content uniformity for NIF and AML in their pharmaceutical dosage forms were extremely comparable with those from official and validated procedures.

Highlights: A validated indirect spectrophotometric method for accurate quantification of some 1,4-dihydropyridine drugs using NBS with the aid of PAP. Monitoring of NIF and AML dosage forms' content uniformity as a first tool or evidence for their efficacy and safety after their administration. Greenness evaluation tools, GAPI and AGREEprep, for measuring the environmental friendliness of the recommended method.

Background: Monitoring total acidity during beverage production is crucial for quality control (QC). The standard acid-base titration, though widely used, is slow and generates hazardous waste through the use of acid-base indicators.

Objective: To develop an analysis method for beverage samples to determine total acidity using a natural reagent from butterfly pea flower as the colorimetric reagent.

Methods: The determination of total acidity in beverages was based on the reaction of citric acid with anthocyanin extracted from butterfly pea flowers. The decreased absorbance of anthocyanin was measured at 620 nm. A two-line reverse flow injection manifold was used to perform online dilution of samples.

Results: Under optimal conditions, the calibration curve equation 1/A = 0.03782C + 0.00241 (A = absorbance and C = concentration) was linear over a range of 0.050-0.25% (w/v) citric acid. The LOD and LOQ were 0.0123 and 0.0409% (w/v), respectively. The system achieved a throughput of 120 samples per hour with comparable accuracy and precision to the standard titrimetric method.

Conclusion: The injection of butterfly pea flower extract into beverage samples with online dilution in a reverse flow injection system (FIS) was reported for the first time for the determination of total acidity.

Highlights: Use of a green reagent in the method reflects its alignment with the principles of green analytical chemistry, providing a rapid and straightforward solution.

Background: The flavor theory of Chinese herbal medicines (CHMs) is one of the core theories of traditional Chinese medicine (TCM). Accurate flavor identification of CHMs is essential to guide the clinical application of CHMs.

Objective: To develop a new method for flavor identification of CHMs according to the ingredient information for CHMs.

Methods: It was found that the chemical basis of medicinal flavors was CHM ingredients. We developed a bitter-pungent flavor identification scheme to build a relationship between medicinal flavors and CHM ingredients. We firstly proposed a scientific hypothesis that "CHMs with similar flavors should have a similar chemical basis". To test this scientific hypothesis, we then explored an intelligent algorithm for bitter-pungent flavor identification of CHMs based on the information similarity of CHM ingredients. GC was used to separate the chemical ingredients of CHMs and analyze the ingredient information of CHMs. A distance metric learning algorithm was built to measure the similarity of GC chemical fingerprints. A bitter-pungent flavor identification scheme (BPFI) was proposed to predict the bitter-pungent flavor of CHMs. Finally, a number of experiments were performed to evaluate the identification performance of our scheme.

Results: Compared to classical algorithms, our proposed BPFI scheme has better flavor prediction performance. The total identification accuracy of our BPFI scheme reached 0.843. The area under ROC (receiver operating characteristic curve) curve (AUC) was 0.899.

Conclusion: The experimental results confirmed our inference that the chemical basis of CHM flavors was CHM ingredients, and implied that CHMs with similar flavors had similar composition. The BPFI model proved to be effective and feasible.

Highlights: Verification hypothesis: CHMs with similar flavors should have similar chemical basis.

Background: Folic acid is an essential nutrient necessary for the synthesis of nucleic acids (DNA and RNA) and certain amino acids. There are no scientifically validated analytical methods for folic acid applicable to all dosage forms.

Objective: A single-laboratory method was validated for the determination of folic acid content in various dietary supplement dosage forms. This method used ultra-performance liquid chromatography/diode-array detector (UPLC/PDA) to determine the folic acid content in dietary supplements in the form of tablets, two-piece capsules, powder drinks, softgels, and gummies.

Method: The ultra-performance liquid chromatography/diode-array detector method was evaluated for linearity, limit of detection (LOD), limit of quantification (LOQ), repeatability, recovery, specificity, and system suitability.

Results: Linearity of the folic acid standard was shown to be linear in the range of 0.45 µg/mL to 7.37 µg/mL. LOD and LOQ of folic acid were 0.089 and 0.268 µg/mL, respectively. The repeatability of nine samples from five matrixes resulted in 1.15-4.82% relative standard deviation (RSD). Five samples with five different matrixes spiked with 25, 50, and 100% of working standard concentration and had a recovery range of 95.48-104.72%. The chromatograms and spectra of the blank, standard, and sample solutions showed that the method was free of interference for folic acid. The system suitability results of different matrixes showed that the UPLC/PDA system is suitable for folic acid analysis. All the AOAC INTERNATIONAL SMPR® 2022.002 requirements were fulfilled.

Conclusions: The ultra-performance liquid chromatography/diode-array detector method compares favorably with the requirements of AOAC SMPR 2022.002.

Highlights: The UPLC/PDA method is fast and suitable for all dietary supplement matrixes studied. The method meets the requirements of SMPR 2022.002.

Background: Caryophyllaceae is a big family composed of many economic and medicinal species. However, the phylogeny of the family is insufficient and genome data are lacking for many species.

Objective: Using next-generation sequencing (NGS) to acquire the chloroplast (cp) genomes of Eremogone acicularis (F.N.Williams) Ikonn., E. brevipetala (Tsui & L.H.Zhou) Sadeghian & Zarre, E. bryophylla (Fernald) Pusalkar & D.K.Singh, E. kansuensis (Maxim.) Dillenb. & Kadereit, Shivparvatia glanduligera (Edgew.) Pusalkar & D.K.Singh, Silene atsaensis (Marq.) Bocquet, S. caespitella Williams, and S. lhassana (Williams) Majumdar.

Methods: Bioinformatic software was used to conduct the comparative genome and phylogeny analysis of these cp genomes.

Results: The eight cp genomes were 132 188-151 919 bp in length, containing 130-132 genes. A/T was dominant in simple sequence repeats (SSRs). Forward repeats and palindromic repeats were the most frequent in long terminal repeats (LTRs). Compared with the four species of Eremogone Fenzl, the inverted repeat (IR) boundaries of S. caespitella, S. atsaensis, S. lhassana, and Sh. glanduligera were significantly expanded. Four and one mutational hotspots were identified in the large single copy (LSC) region and small single copy (SSC) region, respectively. The ratio of nonsynonymous substitution to synonymous substitution (Ka/Ks ratio) showed these cp genomes may have undergone strong purifying selection. In the phylogenetic trees, both Silene L. and Eremogone were monophyletic groups. However, Sh. glanduligera was closely related to Amaranthus hypochondriacus.

Conclusion: These results have provided new evidence and useful information for species identification, evolution, and genetic research on the Caryophyllaceae.

Highlights: In this study, eight newly sequenced cp genomes of Caryophyllaceae species were reported for the first time.