Cyclodextrin-Modified Micellar UPLC for Direct, Sensitive and Selective Determination of Water Soluble Vitamins in Milk

2019 ◽  
Vol 58 (3) ◽  
pp. 203-210
Author(s):  
Hassan M Albishri ◽  
Abdullah M Almalawi ◽  
Wael Alshitari ◽  
Deia Abd El-Hady
Keyword(s):  
Negative Impact ◽  
Stationary Phases ◽  
Bovine Milk ◽  
High Sensitivity ◽  
Water Soluble ◽  
Thiamine Hydrochloride ◽  
Selective Determination ◽  
Milk Samples ◽  
Relative Standard

Abstract Cyclodextrin-modified micellar ultra pressure liquid chromatography (CD-MUPLC) was firstly developed and directly applied to the simultaneous determination of water-soluble vitamins thiamine hydrochloride (VB1), pyridoxine hydrochloride (VB6) and ascorbic acid (VC) in milk samples. A hybrid isocratic mobile phase consisting of β-cyclodextrin (β-CD, 5.0 mmol L−1) and cetyltrimethylammonium bromide (CTAB, 0.1 mol L−1) in the presence of acetic acid (0.1 mol L−1) at pH 2.9 on a RP-C18 column at 25.0°C was successfully used. The separation of vitamins was achieved in less than 10 min at a 0.2 mL min−1 flow rate showing adequate linearity at 245 nm in the ranges of 5.0–500.0 μg L−1 for VB1, 5.0–1000.0 μg L−1 for VB6 and 5.0–10000.0 μg L−1 for VC with coefficients of variation (r2) of 0.9999, 0.9987 and 0.9971, respectively. In addition, limits of detection obtained were 0.885, 1.352 and 1.358 μg L−1 and limits of quantification were 2.681, 4.096 and 4.115 μg L−1 for VB1, VB6 and VC, respectively. The high sensitivity of the proposed CD-MUPLC-UV method permitted its applications to the determination of water-soluble vitamins VB1 (32–488 μg L−1), VB6 (82–95 μg L−1) and VC (790–45000 μg L−1) in breast and bovine milk samples. The relative standard deviations and recoveries ranged between 0.07 and 2.14% and between 85.27 and 114.8%, respectively, indicating the accurate and precise measurements without any negative impact of matrix. The current analytical method illustrated several advantages including direct, sensitive, selective and non-consuming organic solvents over the hitherto published methods. These features could be attributed to the four-point competitive interactions among analytes, pseudostationary phases and modified C18 stationary phases.

scholarly journals Bacterial identification, somatic cell count, antimicrobial profile and toxigenic Staphylococcus strains search from mastitic cow milk samples on small farms properties

2019 ◽  
Vol 39 (9) ◽  
pp. 715-722
Author(s):  
Ubirajara L. Lavor ◽  
Felipe F. Guimarães ◽  
Anelise Salina ◽  
Mateus S.R. Mioni ◽  
Helio Langoni
Keyword(s):  
Public Health ◽  
Somatic Cell ◽  
Negative Impact ◽  
Bovine Milk ◽  
Bovine Mastitis ◽  
High Sensitivity ◽  
Cow Milk ◽  
Small Farms ◽  
Milk Samples ◽  
Cell Counts

ABSTRACT: Bovine mastitis has a negative impact on milk production and can pose risks to public health. The present study aimed to evaluate the quality of bovine milk from small farms in the Botucatu/SP region. Somatic cell counts (SCC), identification of pathogens involved in mastitis, and sensitivity antimicrobial profile of staphylococci isolated were performed. The presence of enterotoxin encoding genes in isolates of staphylococci obtained from milk was investigated. Milk samples from individual mammary quarters of cows were submitted to the California mastitis test (CMT) and SCC. Of the 239 dairy cows from 21 dairy herds evaluated (mean = 11.4 animals/property), two cows (0.8%) presented clinical mastitis and 86 (35.9%) subclinical mastitis. Bacterial culture was performed in 177 quarter milk samples. Staphylococci were identified in 55 (31.1%), corynebacteria in 45 (25.4%), streptococci in 25 (14.1%) and coliforms in four (2.3%) milk samples. Average SCC from culture-positive samples was 1598x103 cells/mL, in case of staphylococci was 1362x103 cells/ml, streptococci was 2857x103 cells/mL, corynebacteria was 976x103 cells/mL and in the cases of coliforms 1161x103 cells/mL were obtained. Staphylococci showed a high sensitivity (>95%) to cephalothin, cotrimoxazole, enrofloxacin, and gentamicin, with a 41.2% resistance to penicillin and 11.8% to oxacillin. Both coagulase positive (CPS) and negative staphylococci (CNS) carried genes encoding enterotoxins in 21.6% of the first group and 41.9% in the second. The sea gene was the most detected 45.8% (n=24) between them, followed by seb with 29.2% and sec with 25.0%. The sed gene was not identified. We highlight the potential risk to public health in the possibility of strains of Staphylococcus spp. enterotoxin-producing genes that can cause staphylococcal food poisoning.

Atomic absorption determination of Hg (II), Cd (II), and As (III) in natural and waste water after preliminary group preconcentration

2019 ◽  
Vol 85 (2) ◽  
pp. 12-16
Author(s):  
I. V. Saunina ◽  
E. N. Gribanov ◽  
E. R. Oskotskaya
Keyword(s):  
Waste Water ◽  
Atomic Absorption ◽  
High Sensitivity ◽  
Distribution Coefficients ◽  
Neutral Medium ◽  
Atomic Absorption Determination ◽  
Absorption Determination ◽  
Relative Standard ◽  
Preliminary Group

The sorption of Hg (II), Cd (II), and As (III) by natural aluminosilicate is studied. It is shown that the mineral absorbs those toxicants in a rather wide pH range, quantitative extraction of analytes being achieved in a neutral or close to neutral medium (pH values range within 7.0 - 8.0; 6.3 - 7.5; 7.4 - 8.5 for Hg (II), As (III), and Cd (II), respectively). The effect of the time of phase contact on the degree of extraction of elements is shown. The sorption capacity of the mineral in optimal conditions of the medium acidity (0.06 mmol/g for mercury, 0.31 mmol/g for cadmium, and 0.52 mmol/g for arsenic) is determined. The distribution coefficients attain values of aboutnX 103-nX 104. A new combined method for determination of Hg (II), Cd (II), and As (III) in natural and waste water is developed and tested. The method consists in a preliminary group sorption concentration of the analytes by aluminosilicate, desorption of the analytes from the surface of the mineral and their subsequent atomic absorption determination. The correctness of the method is verified in analysis of spiked samples. The method is easy to use and exhibits high sensitivity, reproducibility and accuracy of analyte determination. The relative standard deviation does not exceed 0.13. Economic availability and possibility of using domestic sorption materials are the important advantages of the proposed procedure which can be used in the practice of laboratories monitoring the quality and safety of environmental objects.

Fluorometric determination of uric acid in bovine milk

2010 ◽  
Vol 77 (4) ◽  
pp. 438-444 ◽  
Author(s):  
Torben Larsen ◽  
Kasey M Moyes
Keyword(s):  
Heat Treatment ◽  
Uric Acid ◽  
Xanthine Oxidase ◽  
Bovine Milk ◽  
Oxidase Inhibitor ◽  
Enzymatic Oxidation ◽  
Fast Method ◽  
Xanthine Oxidase Inhibitor ◽  
Milk Samples

The primary objective of this study is to validate a new fast method for determination of uric acid in milk. The method is based on an enzymatic-fluorometric technique that requires minimal pre-treatment of milk samples. The present determination of uric acid is based on the enzymatic oxidation of uric acid to 5-hydroxyisourate via uricase where the liberated hydrogen peroxide reacts with 10-acetyl-3,7-dihydroxyphenoxazine via peroxidase and the fluorescent product, resorufin, is measured fluorometrically. Fresh composite milk samples (n=1,072) were collected from both Jersey (n=38) and Danish Holstein (n=106) cows from one local herd. The average inter- and intra-assay variations were 7·1% and 3·0%, respectively. Percent recovery averaged 103·4, 107·0 and 107·5% for samples spiked with 20, 40 or 60 μmof standard, respectively, with a correlation (r=0·98;P<0·001) observed between the observed and expected uric acid concentrations. A positive correlation (r=0·96;P<0·001) was observed between uric acid concentrations using the present method and a reference assay. Storage at 4°C for 24 h resulted in lower (P<0·01) uric acid concentrations in milk when compared with no storage or samples stored at −18°C for 24 h. Addition of either allopurinol (a xanthine oxidase inhibitor) or dimethylsulfoxide (a solvent for allopurinol) did not affect milk uric acid concentrations (P=0·96) and may indicate that heat treatment before storage and analysis was sufficient to degrade xanthine oxidase activity in milk. No relationship was observed between milk uric acid and milk yield and milk components. Authors recommend a single heat treatment (82°C for 10 min) followed by either an immediate analysis of fresh milk samples or storage at −18°C until further analysis.

scholarly journals Simultaneous Determination of C18 Fatty Acids in Milk by GC-MS

Separations ◽  
2021 ◽  
Vol 8 (8) ◽  
pp. 118
Author(s):  
Meiqing Chen ◽  
Yangdong Zhang ◽  
Fengen Wang ◽  
Nan Zheng ◽  
Jiaqi Wang
Keyword(s):  
Fatty Acids ◽  
High Sensitivity ◽  
Raw Milk ◽  
Uht Milk ◽  
Milk Samples ◽  
Accuracy And Precision ◽  
Different Temperatures ◽  
Chromatographic Resolution ◽  
Commercial Milk

The determination of C18 fatty acids (FAs) is a key and difficult aspect in FA profiling, and a qualified method with good chromatographic separation and high sensitivity, as well as easy methylation, is required. A GC-MS method was established to simultaneously determine C18 FAs in milk. To simplify the methylation protocol for milk samples, besides a base-catalyzation methylation (50 °C for 20 min), the necessity of an additional acid-catalyzation was also studied using different temperatures (60 °C, 70 °C, 80 °C, and 90 °C) and durations (90 min and 150 min). The results showed that the chromatographic resolution was improved, although three co-eluted peaks existed. The base-catalyzation was sufficient, and an additional acid-catalyzation was not necessary. The proposed method was validated with good sensitivity, linearity, accuracy, and precision, and then applied in determining C18 FAs in 20 raw milk and 30 commercial milk samples. UHT milk presented a different profile of C18 FAs from raw milk and PAS milk samples, which indicated that excessive heating could change the profile. Overall, the proposed method is a high-throughput and competent approach for the determination of C18 FAs in milk, and which presents an improvement in chromatographic resolution and sensitivity, as well as a simplification of methylation.

scholarly journals New Spectrofluorimetric Method with Enhanced Sensitivity for Determination of Paroxetine in Dosage Forms and Plasma

2008 ◽  
Vol 3 ◽  
pp. ACI.S1053 ◽  
Author(s):  
Ibrahim A. Darwish ◽  
Sawsan M. Amer ◽  
Heba H. Abdine ◽  
Lama I. Al-Rayes
Keyword(s):  
High Sensitivity ◽  
Dosage Forms ◽  
Official Method ◽  
Factors Affecting ◽  
Pharmaceutical Tablets ◽  
Enhanced Sensitivity ◽  
Spectrofluorimetric Method ◽  
Relative Standard ◽  
Optimized Conditions

New simple spectrofluorimetric method with enhanced sensitivity has been developed and validated for the determination of the antidepressant paroxetine (PXT) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of PXT with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 545 nm after excitation at 490 nm. The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient (0.9993) was found between the fluorescence intensity and PXT concentration in the range of 80-800 ng ml-1. The limits of detection and quantitation for the method were 25 and 77 ng ml-1, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 3%. The proposed method was successfully applied to the determination of PXT in its pharmaceutical tablets with good accuracy; the recovery values were 100.2 ± 1.61%. The results obtained by the proposed method were comparable with those obtained by the official method. The proposed method is superior to the previously reported spectrofluorimetric method for determination of PXT in terms of its higher sensitivity and wider linear range. The high sensitivity of the method allowed its successful application to the analysis of PXT in spiked human plasma. The proposed method is practical and valuable for its routine application in quality control and clinical laboratories for analysis of PXT.

scholarly journals Determination of Four Fluoroquinolones in Milk by Liquid Chromatography

1997 ◽  
Vol 80 (5) ◽  
pp. 982-987 ◽  
Author(s):  
José E Roybal ◽  
Allen P Pfenning ◽  
Sherri B Turnipseed ◽  
Calvin C Walker ◽  
Jeffrey A Hurlbut
Keyword(s):  
Fluorescence Detection ◽  
Solid Phase ◽  
Raw Milk ◽  
Extraction Column ◽  
Isocratic Elution ◽  
Standard Curve ◽  
Milk Samples ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method with fluorescence detection is presented for the analysis of 4 fluoroquinolones; enrofloxacin (ENRO), ciprofloxacin (CIPRO), sarafloxacin (SARA), and difloxacin (DIFLX) in milk. The procedure consists of extraction of milk with acidified ethanol, isolation and retention on a cation exchange solid-phase extraction column, elution with basic methanol, and LC analysis with fluorescence detection. LC analysis is performed by isocratic elution using an acetonitrile-2% acetic acid (15 + 85) mobile phase and an Inertsil phenyl column with fluorescence detection at excitation and emission wavelengths of 278 and 450 nm, respectively. A target level of 10 ppb for each of the 4 fluoroquinolones has been established for this method. Average recovery from fortified raw milk samples (5-100 ppb each) based on a 5-point standard curve calculation was 70-90%, with relative standard deviations of &lt;15%.

scholarly journals Determination of carcinogenic herbicides in milk samples using green non-ionic silicone surfactant of cloud point extraction and spectrophotometry

2018 ◽  
Vol 5 (4) ◽  
pp. 171500 ◽  
Author(s):  
N. I. Mohd ◽  
N. N. M. Zain ◽  
M. Raoov ◽  
S. Mohamad
Keyword(s):  
Cloud Point ◽  
Cloud Point Extraction ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Silicone Surfactant ◽  
Extraction Solvent ◽  
Milk Samples ◽  
Relative Standard ◽  
Limit Of Quantitation

A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient ( R 2 ) in the range of 0.991–0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l −1 (atrazine) and 1.22 µg l −1 (propazine), and the limit of quantitation was 3.54 µg l −1 (atrazine) and 4.07 µg l −1 (propazine). Satisfactory recoveries in the range of 81–108% were determined in milk samples at 5 and 1000 µg l −1 , respectively, with low relative standard deviation, n  = 3 of 0.301–7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.

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