Advancements and greenification potential of magnetic molecularly imprinted polymers for chromatographic analysis of veterinary drug residues in milk.

Milk, as a widely consumed nutrient-rich food, is crucial for bone health, growth, and overall nutrition. The persistent application of veterinary drugs for controlling diseases and heightening milk yield has imparted substantial repercussions on human health and environmental ecosystems. Due to the high demand, fresh consumption, complex composition of milk, and the potential adverse impacts of drug residues, advanced greener analytical methods are necessitated. Among them, functional materials-based analytical methods attract wide concerns. The magnetic molecularly imprinted polymers (MMIPs), as a kind of typical functional material, possess excellent greenification characteristics and potencies, and they are easily integrated into various detection technologies, which have offered green approaches toward analytes such as veterinary drugs in milk. Despite their increasing applications and great potential, MMIPs' use in dairy matrices remains underexplored, especially regarding ecological sustainability. This work reviews recent advances in MMIPs' synthesis and application as efficient sorbents for veterinary drug extraction in milk followed by chromatographic analysis. The uniqueness and effectiveness of MMIPs in real milk samples are evaluated, current limitations are addressed, and greenification opportunities are proposed. MMIPs show promise in revolutionizing green analytical procedures for veterinary drug detection, aligning with the environmental goals of modern food production systems.

Comparison of analyte identification criteria and other aspects in triple quadrupole tandem mass spectrometry: Case study using UHPLC-MS/MS for regulatory analysis of veterinary drug residues in liquid and powdered eggs.

Ultrahigh-performance liquid chromatography (UHPLC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) is one of the most powerful tools for the multiclass, multiresidue analysis of veterinary drugs, pesticides, mycotoxins, and other chemical contaminants in foods and other sample types. Until approximately 2010, commercial MS/MS instruments using multiple reaction monitoring (MRM) were generally limited to minimum dwell (and inter-dwell) times of 10 ms per ion transition. To achieve the needed accuracy and detection limits for hundreds of targeted analytes, older UHPLC-MS/MS methods typically acquired only two ion transitions per analyte (yielding only one ion ratio for qualitative identification purposes), which is still the norm despite technological advancements. Newer instruments permit as little as 1 ms (inter-)dwell times to afford monitoring of more MRMs/analyte with minimal sacrifices in accuracy and sensitivity. In this study, quantification and identification were assessed in the validation of 169 veterinary drugs in liquid and powdered eggs. Quantitatively, an "extract-and-inject" sample preparation method yielded acceptable 70-120% recoveries and < 25% RSD for 139-141 (82-83%) of the 169 diverse drug analytes spiked into powdered and liquid eggs, respectively, at three levels of regulatory interest. Qualitatively, rates of false positives and negatives were compared when applying three different regulatory identification criteria in which two or three MRMs/drug were used in each case. Independent of the identification criteria, rates of false positives remained <10% for 95-99% of the drugs whether 2 or 3 ions were monitored, but the percent of drugs with >10% false negatives decreased from 25-45 to 10-12% when using 2 vs. 3 MRMs/analyte, respectively. Use of a concentration threshold at 10% of the regulatory level as an identification criterion was also very useful to reduce rates of false positives independent of ion ratios. Based on these results, monitoring >2 ion transitions per analyte is advised when using MS/MS for analysis, independent of SANTE/12682/2019, FDA/USDA, or 2002/657/EC identification criteria. (Quant)identification results using all three criteria were similar, but the SANTE criteria were advantageous in their greater simplicity and practical ease of use.

Assessment of safety and quality aspects of boiling treatment of quail eggs.

A total of 300 quail eggs were collected randomly from different markets in Cairo and Giza Governorates. Five eggs were represented as one egg sample. Shell and content of each egg were examined for their microbiological contents, sensory evaluation and study of Escherichia coli O157 survival in artificially contaminated eggs. Moreover, qualitative detection of antimicrobial residues by seven plates microbiologically bioassay and confirmed by validated high-performance liquid chromatography (HPLC) methods for positively reacted antimicrobials in raw and boiled samples. There was a significant difference (P < 0·05) between the grading score of eggs after the boiling at 2-, 4-, 5- and 7-min. Based on the survival results, the refrigeration storage and boiling for 5 min of quail eggs was confirmed that such eggs are without E. coli O157. After the boil, the concentrations of oxytetracycline (OTC) and 4-Epi-OTC residues were significantly reduced, and there was no effect on the concentration of sulphadimidine (SDD), amoxicillin (AMO) and Diketo residues. Samples that exceeded the maximum residual limits (MRLs) were 17·0%, 12·0%, 10·0%, 16·0% and 14·0% for SDD, OTC, 4-Epi-OTC, AMO and Diketo, respectively. After boiling, no significant change was noted for SDD, AMO and Diketo, but all OTC and 4-Epi-OTC were completely below MRLs. Therefore, SDD and AMO with their metabolite (Diketo) are heat-stable antimicrobial residues with multiple human health hazards.

Evanescent Wave Optical Fiber Sensors Using Enzymatic Hydrolysis on Nanostructured Polyaniline for Detection of ß-Lactam Antibiotics in Food and Environment.

ß-Lactam antibiotics such as penicillins and cephalosporins are extensively used for human infection therapy. Consistent unintended exposure to these antibiotics via food and water is known to promote antibiotic-resistant bacterial pathogenesis with high morbidity and mortality in humans. An optical enzymatic biosensor for rapid and point-of-use detection of these antibiotics in food and water has been developed and tested. Enzymatic hydrolysis of ß-lactams, on the electroactive polyaniline nanofibers, altered the polymeric backbone of the nanofibers, from emeraldine base form to emeraldine salt, which was measured as an increase in evanescent wave absorbance at 435 nm. The sensors were calibrated by spiking antibiotic-free milk with ceftazidime (as a model ß-lactam analyte) in a linear range of 0.36-3600 nM (R2 = 0.98). The calibration was further validated for packaged milk, local cow milk, and buffalo milk. A similar calibration was devised for chicken meat samples in a linear range of 9-1800 nM (R2 = 0.982) and tap water in a linear range of 0.18-180 nM (R2 = 0.99). Interestingly, it was possible to use the same calibration for the determination of other ß-lactam antibiotics (ampicillin, amoxicillin, and cefotaxime), which reflects the usefulness of the sensor for wide-scale deployment. The sensor performance was validated with a wastewater sample, from a wastewater treatment plant (WWTP), qualitatively analyzed by high-resolution liquid chromatography coupled with mass spectroscopy for detection of ß-lactams. The sensor scheme developed and tested is of grassroot relevance as a quick solution for measurement of ß-lactam residues in food and environment.

Simultaneous determination of 11 quinolone residues in freshwater fish samples by magnetic solid-extraction coupled to liquid chromatography-tandem mass spectrometry.

In this study, well-defined core-shell ethylenediamine-functional magnetic ferroferric oxide polymers were prepared and were fully characterized by transmission electron microscopy, scanning electron microscopy, FTIR spectroscopy, and vibrating sample magnetometry. Then, it was used as a magnetic solid-phase extraction adsorbent for simultaneous determination of 11 trace quinolone residues in freshwater fish samples coupled to liquid chromatography-tandem mass spectrometry. The obtained results revealed that the adsorbent showed good extraction efficiency and the adsorption mechanisms referred to hydrogen bond and π-π stacking interaction. Moreover, the magnetic solid-phase extraction conditions were also carefully optimized. The limits of quantitation of 11 quinolones were in the range of 0.15-0.36 µg/kg, while spiking recoveries were in the range of 80.2-99.5% for the 11 quinolones in freshwater fish samples at four spiked levels including limits of quantitation, 1.0, 40.0, and 80.0 µg/kg with the relative standard deviations ranging from 0.8 to 9.1%. The proposed method was applied to analyze 45 freshwater fish samples, and enrofloxacin was detected in 91.1% samples with concentrations ranging from 0.659 to 333 µg/kg. It could be concluded that the proposed method is fast, simple, sensitive, and accurate for the routine monitor of freshwater fish.

Natural thymol-based ternary deep eutectic solvents: Application in air-bubble assisted-dispersive liquid-liquid microextraction for the analysis of tetracyclines in water.

Four new thymol-based ternary deep eutectic solvents were prepared and evaluated as the extractive phase in air-bubbles assisted dispersive liquid-liquid microextraction for extraction of tetracycline, doxycycline, and oxytetracycline from the water before high-performance liquid chromatography. The maximum extraction efficiencies were obtained using 400 µL of [choline chloride]:[thymol]:[nonanoic acid] in the molar ratio of 1:2:2 at pH = 5. The solvent was characterized by FTIR and NMR spectroscopy. The hydrophobicity of the deep eutectic solvent and its effect on the pH of water samples after mixing was also studied. Besides, the extraction efficiency of the ternary deep eutectic solvent was compared with that of two binary thymol-based deep eutectic solvents, including [choline chloride]:[thymol] and [thymol]:[nonanoic acid] at the same conditions. Under optimal conditions, limits of detection and quantification were 1.2-8.0 and 3.8-26.6 µg/L, respectively. The linear ranges were 18.2-500 µg/L for oxytetracycline, 26.6-500 µg/L for tetracycline, and 3.8-500 µg/L for doxycycline with the determination coefficients > 0.9912. Intra- and inter-day relative standard deviations were 1.2-3.8 and 7.7-11.2%, respectively. The developed method was applied to the analysis of tetracyclines in unspiked and spiked environmental water samples, and the obtained recoveries were 74.5-95.4% with relative standard deviations of 1.2-4.0%.

Monitoring the behavior of imazalil and its metabolite in grapes, apples, and the processing of fruit wine at enantiomeric level.

BACKGROUND: Imazalil is widely used in agriculture, which may pose a threat to food safety. This study aimed to investigate the fate of imazalil and its main metabolite, R14821 (imazalil-M), in field grapes and apples, and in the processing of fruit wine at the enantiomeric level. RESULTS: Analysis method was established to determine imazalil and imazalil-M enantiomers in grape, apple, fruit wine and pomace. The method showed acceptable recoveries of 71.6-99.9% and precision with relative standard deviation of 0.3-11.7%. Processing factors (PFs) were 0.15-0.40 (for imazalil enantiomers) and <0.13-0.83 (for imazalil-M enantiomers) during the wine-making process. The PFs after individual steps including washing, peeling, fermentation, and clarification were all less than 1. No enantioselective dissipation of imazalil was found in grapes under field conditions with half-lives of 23.82-24.49 days. R-(-)-imazalil degraded slightly faster than S-(+)-imazalil in apples under field conditions with half-lives of 9.82-10.09 days. S-(+)-imazalil-M preferentially degraded in field grapes and apple. No significant enantioselectivity of imazalil and imazalil-M was observed during the wine-making process. The enantiomeric fraction (EF) values of imazalil were 0.484-0.511 and 0.509-0.522 in grape wine and cider, respectively. The EFs were 0.484-0.501(in grape wine) and 0.484-0.504 (in cider) for imazalil-M. CONCLUSION: The results showed that the wine-making process could reduce imazalil and imazalil-M residues in grapes and apples. The finding of non-enantioselectivity of imazalil during the processing of fruit wine was useful for accurate risk assessment for imazalil in raw and processing fruits. © 2021 Society of Chemical Industry.

Preparation of porous magnetic molecularly imprinted polymers for fast and specifically extracting trace norfloxacin residue in pork liver.

Here, magnetic molecularly imprinted polymers were designed for norfloxacin via oil-in-water emulsifier-free emulsion method. It was prepared by simply mixing norfloxacin, methacrylic acid-co-ethylene glycol dimethacrylate copolymer, and Fe3 O4 together at room temperature. Characterized by multiple analytical tools, the particle size, pore size, pore volume, specific surface area, and saturation magnetization of the product were about 30 µm, 10-500 nm, 2.92 mL/g, 105.84 m2 /g, and 3.052 emu/g, respectively. And the adsorption capacity was high at 27.04 mg/g towards norfloxacin. Combined with ultra high performance liquid chromatography, it was used to determine norfloxacin in real samples. Average recoveries were above 77.44% with relative standard deviations between 1.21 and 6.85% at three spiked levels (n = 3) for lake water and pork liver. The determination was achieved for the most complex biosample pork liver spiked with norfloxacin low to 30 ng/g, about 100 times less than the maximum residue limit regulated by Commission of the European Communities. All evidences demonstrated that the magnetic molecularly imprinted polymers can be used in practice for monitoring norfloxacin either in environmental water or meat product with high accuracy and reliability.

Simultaneous determination of multiclass plant growth regulators in fruits using the quick, easy, cheap, effective, rugged, and safe method and ultra-high performance liquid chromatography-tandem mass spectrometry.

In this study, a modified quick, easy, cheap, effective, rugged, and safe method combined with ultra-high performance liquid chromatography and tandem mass spectrometry was developed for the multiclass determination of 28 plant growth regulators in various fruits. Different extraction solvents and adsorbents, including primary secondary amine, octadecylsilyl, graphitized carbon black, and zirconia-based sorbent, were investigated. Internal calibration and isotope internal standards, chlormequat chloride-d4 , mepiquat chloride-d6 , indole-3-acetic acid-d2 , and forchlorfenuron-d5 were used to improve accuracy. For method validation, good linearity, low limits of detection and quantification were obtained. At three spiked concentrations (10, 50, and 100 µg/kg), satisfactory recoveries with relative standard deviations of 2.4-17.5% were obtained for strawberries (75.2-119.8%), grapes (70.5-114.0%), tangerines (71.7-115.4%), apples (72.7-115.4%), and kiwi fruits (71.7-119.2%). Samples analysis revealed that 15.6% of the samples (n = 96) were contaminated with one or two kinds of plant growth regulators, including chlormequat chloride, forchlorfenuron, paclobutrazol, 2,4-dichlorophenoxyacetic acid, 2-diethylaminoethyl hexanoate, and mepiquat chloride. Similar results were obtained by ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry, indicating the robustness, effectiveness, and suitability of the developed method for routine monitoring of plant growth regulator residues in fruits.

The determination of ß-agonist residues in bovine tissues using liquid chromatography-tandem mass spectrometry.

We aimed to develop a rapid, simple and reproducible method based on LC-tandem mass spectrometry (LC-MS/MS) to analyze ß-agonist residues (clenbuterol, zilpaterol, ractopamine and isoxsuprine) in bovine tissues. The method was validated in accordance with the European Council Decision 2002/657/EC. The samples were homogenized, and then 10 mL of an acetate buffer was added to a 5-g sample. The sample was then centrifuged at 12,000 rpm and filtered. Sodium hydroxide (2 m) was added to adjust pH of the sample that was centrifuged again. The extract was filtered through a solid-phase extraction column. The residue was re-dissolved in 250 µL acetonitrile and then subjected to LC-MS/MS. The separation was done on a C18 column. The mobile phase consisted of 0.1% formic acid in deionized water and 0.1% formic acid in methanol. The mean recoveries of ß-agonists were in the range of 84.3%-119.1% with relative standard deviations (%RSDs) of 0.683%-4.05%. Decision limits and detection capabilities of the analytes ranged from 0.0960 to 4.9349 µg/kg and from 0.0983 to 5.0715, respectively. This method was used to detect four ß-agonists in 100 bovine muscle, 100 liver and 100 kidney tissues from a slaughterhouse. No residue was found above the maximum residue limit level.

Short communication: Anesthetic residues in milk after topical application during treatment of hoof lesions in dairy cows.

Hoof lesions in dairy cows are usually treated by trimming the hoof. However, trimming by itself can cause severe pain or exacerbate already existing pain. Hoof trimming is usually not carried out by trained veterinarians, and pain management is not provided. Pain control during trimming is not only an ethical obligation but also allows for better manipulation and more meticulous treatment. Tri-Solfen (Bayer Animal Health, Pymble, Australia) is a spray gel containing lidocaine, bupivacaine, and cetrimide that is easily applied topically and has demonstrated pain-mitigation effects during and after hoof trimming. In the European Union, these local anesthetics are not approved for use in food-producing animals because of a lack of residue data and concerns about genotoxic effects in cattle and humans. The aim of this study was to assess lidocaine, bupivacaine, and 2,6-xylidine residues in milk after Tri-Solfen application in dairy cows. Five dairy cattle in the dry-off period were enrolled in the study based on clinical evidence of lameness (score ≥3 on a 5-point scale). After cleaning and superficial trimming, we applied 3 to 14 mL of Tri-Solfen to the lesions before continuing treatment. Two milk samples were collected per animal in the following 4 milkings and analyzed in a reference laboratory. Residues of lidocaine above the limits of quantification (0.2 µg/L) were found in milk samples in the first milking 6 h after treatment in only 2 cows. This study shows that excretion of local anesthetics and their metabolites in milk after topical application of Tri-Solfen is negligible and even undetectable after the first milking 6 h post-treatment.

Oestrogens in milk and breast cancer: a cause for concern or not?

In this short Research Reflection I address and refute the suggestion that oestrogens consumed in milk might contribute in a significant way to endogenous levels and thereby have a physiological action, possibly resulting in adverse consequences including increased breast cancer risk. Quantitative analysis based on published data shows that, even in worst case scenarios, oestrogen consumption in milk is considerably less than regulatory bodies regard as entirely safe.

Microbiological and physicochemical characteristics of buffalo milk used for dairy products in southern Brazil.

In Brazil, the buffalo milk market has been growing. However, identity and quality standards have not been established for this raw material, nor have proper distinctions between buffalo milk and bovine milk been defined. Currently, the State of Rio Grande do Sul (RS) has only three producers that supply raw material for officially marketed derivatives. The aim of this study was to determine the identity and quality standards of raw buffalo milk in this region. Samples were obtained biweekly from three farm cooling tanks between June 2017 and August 2018, to reach a total of 69 samples. The averages for the results of the physicochemical parameters fat, protein, lactose, total solids, SNF (solids-not-fat), calcium, density, FP, acidity and SCC were 5.5 g/100 g, 4.06 g/100 g, 5.07 g/100 g, 15.5 g/100 g, 9.96 g/100 g, 0.161 g/100 g, 1.034 g/ml, -0.527°C, 16°D and 95 × 103 cells/ml, respectively. With reference to the microbiological parameters, the mean of the Standard Plate Count (SPC) and thermotolerant coliforms were 9,0 × 104 CFU/ml and 1.6 × 102 MPN/ml, respectively. Regarding coagulase-positive staphylococci, 36 samples tested positive (52% of total). Neither Salmonella spp. nor Listeria monocytogenes, nor antibiotic or antiparasitic residues were detected in any sample. In conclusion, the buffalo milk used as raw material for dairy products in southern Brazil demonstrated satisfactory physicochemical and microbiological characteristics, in accordance with recent scientific literature.

Ultrasonication-facilitated synthesis of functionalized graphene oxide for ultrasound-assisted magnetic dispersive solid-phase extraction of amoxicillin, ampicillin, and penicillin G.

A simplistic approach is presented for the synthesis of ultrasonically fabricated graphene oxide functionalized with polyaniline and N-[3-(Trimethoxysilyl)propyl]ethylenediamine. The synthesized nanocomposite was then employed for the facile, green, ultrasound-assisted, magnetic dispersive solid-phase extraction of amoxicillin, ampicillin, and penicillin G in milk samples and infant formula prior to high-performance liquid chromatography-ultraviolet determination. The designed nanocomposites were comprehensively characterized using field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, X-ray powder diffraction, and Fourier transform infrared spectroscopy. In order to achieve the best extraction efficiencies, the influential parameters including pH, amount of magnetic sorbent, type and volume of elution solvent, extraction time, sample volume, and desorption time were assessed. At the optimum conditions, linear ranges of 2.5-1000 (µg L-1) for ampicillin and penicillin G and a linear range of 2.5-750 (µg L-1) were obtained for amoxicillin at optimum conditions. Moreover, the limits of detection (S/N = 3) of 0.5, 0.8, and 0.9 (µg L-1) were obtained for amoxicillin, ampicillin, and penicillin G, respectively. The precision (relative standard deviations (%)) values of 3.1, 2.6, and 2.5 at the concentration of 50 µg L-1 for seven replicates were obtained for ampicillin, amoxicillin, and penicillin G, respectively. The efficiencies of ≤ 96% and relative standard deviations of less than 3.1% were also obtained thereby confirming the high potential of the synthesized nanocomposites for simultaneous preconcentration and separation of the ß-lactam antibiotics in complex matrixes. Graphical Abstract.

Determination of Polypeptide Antibiotic Residues in Food of Animal Origin by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry.

A novel UHPLC-MS/MS method for the determination of polypeptide antibiotic residues in animal muscle, milk, and eggs was developed and validated. Bacitracin A, colistin A, colistin B, polymyxin B1, and polymyxin B2 were extracted from the samples with a mixture of acetonitrile/water/ammonia solution 25%, 80/10/10 (v/v/v), and put through further evaporation, reconstitution, and filtration steps. The chromatographic separation was performed on a C18 column in gradient elution mode. Mass spectral acquisitions were performed in selective multiple reaction monitoring mode by a triple quadrupole mass spectrometer. The method was validated according to the criteria of Commission Decision 2002/657/EC. The method quantifies polypeptides in a linear range from 10 to 1000 µg kg-1, where the lowest concentration on the calibration curve refers to the limit of quantification (LOQ). The recoveries ranged from 70 to 99%, the repeatability was below 13%, and within-laboratory reproducibility was lower than 15%. The decision limit (CCα) and detection capability (CCß) values were calculated, and ruggedness and stability studies were performed, to fulfill the criteria for confirmatory methods. Moreover, the developed method may also be used for screening purposes by its labor efficiency.

Dissipation, residues and risk assessment of pyraclostrobin and picoxystrobin in cucumber under field conditions.

BACKGROUND: Pyraclostrobin and picoxystrobin are two representative pesticides of strobilurins used to treat cucumber downy mildew, which have raised issues of food safety and human health. A new formulation containing these two compounds is being prepared for marketing in China. RESULTS: The dissipation and residual levels of pyraclostrobin and picoxystrobin in cucumbers under field conditions were determined simultaneously by a validated method via liquid chromatography-tandem mass spectrometry (LC-MS/MS). The dissipation rules were described by first-order kinetics and the half-lives of pyraclostrobin and picoxystrobin were less than 8.2 days and 3.4 days. The highest terminal residue of pyraclostrobin was 0.014 mg kg-1 which was lower than maximum residue limit (MRL) in China (0.5 mg kg-1 ) and of picoxystrobin was 0.029 mg kg-1 , respectively. In the long-term intake risk assessment of pyraclostrobin and picoxystrobin for general population (18-79 years), the chronic risk quotient (RQc ) varied from 5.64% to 21.97%. The assessment of short-term risks included children (1-6 years) and adults (18-79 years) and in which the RQa values were 0.38% and 2.85%. Both results showed the intake risks of cucumber were acceptable. CONCLUSION: Pyraclostrobin and picoxystrobin degraded easily in cucumbers under open field conditions. The long-term and short-term risks caused by final residues of pyraclostrobin and picoxystrobin were insignificant. The recommended pre-harvest interval of 3 days was safe. The article will be helpful in rational use of these pesticides and MRL formulation of picoxystrobin on cucumber. © 2020 Society of Chemical Industry.

Investigations into the performance of travelling wave enabled conventional and cyclic ion mobility systems to characterise protomers of fluoroquinolone antibiotic residues.

RATIONALE: Fluoroquinolones (FLQs) have been shown to form protomers with distinctive fragment profiles. Experimental parameters affect protomer formation, impacting observed conventional tandem mass spectrometric (MS/MS) dissociation and multiple reaction monitoring (MRM) transition reproducibility. Collision cross section (CCS) measurement can provide an additional identification metric and improved ion mobility (IM) separation strategies could provide further understanding of fluctuations in fragmentation when using electrospray ionisation (ESI). METHODS: Porcine muscle tissue was fortified with nine fluoroquinolone antibiotics. Extracts were cleaned using QuEChERS dispersive extraction. Separation was achieved via ultra-high-performance liquid chromatography (UHPLC) and analysis performed using positive ion ESI coupled with linear T-wave IM (N2 and CO2 drift gas) and cyclic IM-MS (calibrated to perform accurate mass and CCS measurement). RESULTS: IM-resolved protomeric species have been observed for nine FLQs (uniquely three for danofloxacin). Long-term reproducibility and cross-platform T-wave/cIM studies have demonstrated CCS metric errors <1.5% when compared with a FLQ protomer reference CCS library. When comparing FLQ protomer separation using a standard, linear T-wave IM separator (N2 /CO2 ) and using a high-resolution cyclic T-wave device (N2 ), protomer peak-to-peak resolution ranged between Rs = 1 to Rs = 6 for the IM strategies utilised. CONCLUSIONS: CCS is a reliable cross platform metric; specific FLQ CCS identification fingerprints have been produced, illustrating the potential to compliment MS/MS specificity or provide an alternative identification metric. Using cIM there is opportunity to correlate the erratic nature of protomer formation with the analytical conditions used and to gain further understanding of ionisation/dissociation mechanisms taking place during routine analyses.

Instrumental and sensory methodologies to characterize the residual film of topical products applied to skin.

BACKGROUND: The work is aimed at the development of a methodology to characterize the tactile properties of topical products during application. Specific attention was paid to the study of the residual properties left at the surface of the skin. This approach was interestingly used to better understand the formulation factors governing the skinfeel of topical preparations. MATERIALS AND METHODS: Cosmetic and pharmaceutical topical products were selected based on their various texture, galenic form (gel or emulsion), and composition (polymer used as texturing agent). Key texture attributes namely Firmness, Stickiness, Spreadability, and Amount of residue were objectively evaluated using sensory analysis. Additionally, texture analysis (compression test), rheology (flow test), and tribology (in vivo friction test) were carried out. RESULTS: Sensory evaluations highlighted a great diversity of tactile properties among products when applied to skin. For example, assessors perceived an important amount of residue left by emulsions whereas gels were not leaving any residue after application to the skin. These results were confirmed by in vivo tactile friction measurements with two distinct evolutions in time of the residual film properties. CONCLUSION: The present investigation shows how the tactile properties of topical gels and emulsions are studied using complementary tests in order to understand and improve the skinfeel of topical preparations.

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography-tandem mass spectrometry.

We developed an analytical method using liquid-liquid extraction (LLE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) to detect and quantify tebufenozide (TEB) and indoxacarb (IND) residues in animal and aquatic products (chicken muscle, milk, egg, eel, flatfish, and shrimp). The target compounds were extracted using 1% acetic acid (0.1% acetic acid for egg only) in acetonitrile and purified using n-hexane. The analytes were separated on a Gemini-NX C18 column using (a) distilled water with 0.1% formic acid and 5 mm ammonium acetate and (b) methanol with 0.1% formic acid as the mobile phase. All six-point matrix-matched calibration curves showed good linearity with coefficients of determination (R2 ) ≥0.9864 over a concentration range of 5-50 µg/kg. Intra- and inter-day accuracy was expressed as the recovery rate at three spiking levels and ranged between 73.22 and 114.93% in all matrices, with a relative standard deviation (RSD, corresponding to precision) ≤13.87%. The limits of quantification (LOQ) of all target analytes ranged from 2 to 20 µg/kg, which were substantially lower than the maximum residue limits (MRLs) specified by the regulatory agencies of different countries. All samples were collected from different markets in Seoul, Republic of Korea, and tested negative for tebufenozide and indoxacarb residues. These results show that the method developed is robust and may be a promising tool to detect trace levels of the target analytes in animal products.

Validation of strip tests for the rapid screening of ethanol residues in milk.

The experiments reported in this Research Communication aimed to determine if a domestic strip test to detect ethanol residues in breast milk (Milkscreen®) is comparable to a previously established official method for detecting ethanol residues in milk. The two methods are examined in terms of overall sensitivity, robustness against storage and acidity and selectivity against formaldehyde residues. Here, Milkscreen® provided advantages, with faster results (2 min), good sensitivity (≥0.017%), no false results due formaldehyde residues and equal robustness against storage, but with lower sensitivity in acid milk samples. In summary, strip tests for the rapid detection of ethanol residues in breast milk can be used for screening purposes by dairy manufacturers, combining it with the official method to make a final diagnosis.