scholarly journals Multi-Target Analysis and Suspect Screening of Xenobiotics in Milk by UHPLC-HRMS/MS

Separations ◽  
2021 ◽  
Vol 8 (2) ◽  
pp. 14
Author(s):  
Mikel Musatadi ◽  
Belén González-Gaya ◽  
Mireia Irazola ◽  
Ailette Prieto ◽  
Nestor Etxebarria ◽  
...  
Keyword(s):  
Breast Milk ◽  
High Performance ◽  
Biological Fluids ◽  
Food Additives ◽  
Screening Methods ◽  
Target Analysis ◽  
Adverse Health Effects ◽  
Milk Samples ◽  
Anhydrous Na2so4 ◽  
Target Screening

The development of suspect or non-target screening methods to detect xenobiotics in biological fluids is essential to properly understand the exposome and assess its adverse health effects on humans. In order to fulfil that aim, the biomonitorization of human fluids is compulsory. However, these methods are not yet extensively developed, especially for polar organic xenobiotics in biofluids such as milk, as most works are only focused on certain analytes of interest. In this work, a multi-target analysis method to determine 245 diverse xenobiotics in milk by means of Ultra High Performance Liquid Chromatography (UHPLC)-qOrbitrap was developed. Under optimal conditions, liquid milk samples were extracted with acetonitrile in the presence of anhydrous Na2SO4 and NaCl, and the extracts were cleaned-up by protein precipitation at low temperature and Captiva Non-Drip (ND)—Lipids filters. The optimized method was validated at two concentration-levels (10 ng/g and 40 ng/g) obtaining satisfactory figures of merit for more than 200 compounds. The validated multi-target method was applied to several milk samples, including commercial and breast milk, provided by 4 healthy volunteers. Moreover, the method was extended to perform suspect analysis of more than 17,000 xenobiotics. All in all, several diverse xenobiotics were detected, highlighting food additives (benzothiazole) or phytoestrogens (genistein and genistin) in commercial milk samples, and stimulants (caffeine), plasticizers (phthalates), UV filters (benzophenone), or pharmaceuticals (orlistat) in breast milk samples.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S. Zamzam ◽  
Mona H. Abdel Rahman ◽  
Maha F. Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 > 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with <25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S Zamzam ◽  
Mona H Abdel Rahman ◽  
Maha F Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Abstract Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 &gt; 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with &lt;25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

Detection of Aflatoxin M1 in Human Breast Milk and Raw Cow's Milk in Istanbul, Turkey

2009 ◽  
Vol 72 (4) ◽  
pp. 885-889 ◽  
Author(s):  
YAŞAR KESKIN ◽  
RUHTAN BAŞKAYA ◽  
SEHER KARSLI ◽  
TÜRKAN YURDUN ◽  
OĞUZ ÖZYARAL
Keyword(s):  
Breast Milk ◽  
High Performance ◽  
Aflatoxin M1 ◽  
Cow’S Milk ◽  
Enzyme Linked Immunosorbent Assay ◽  
Human Breast Milk ◽  
Human Breast ◽  
Cow's Milk ◽  
Milk Samples ◽  
Raw Cow’S Milk

This survey was undertaken to determine the extent of aflatoxin M1 (AFM1) contamination in human breast milk and raw cow's milk in Istanbul, Turkey. Samples of human and raw cow's milk were collected randomly and analyzed for AFM1 using an enzyme-linked immunosorbent assay and high-performance liquid chromatography with fluorescence detection in which the samples were cleaned up with immunoaffinity columns. In this study, AFM1 was detected in 8 (13.1%) of 61 human breast milk samples examined (mean ± SD level, 5.68 ± 0.62 ng/liter; range, 5.10 to 6.90 ng/liter) and 20 (33.3%) of 60 raw cow's milk samples examined (range, 5.40 to 300.20 ng/liter). Five (8.3%) of the positive raw cow's milk samples had AFM1 levels (153.52 ± 100.60 ng/liter; range, 61.20 to 300.20 ng/liter) that were higher than the maximum tolerance limit (0.05 ppb) stipulated by regulations in Turkey and some other countries.

Evaluation of Commercial Immunochemical Assays for Detection of Sulfamethazine in Milk

1992 ◽  
Vol 55 (4) ◽  
pp. 284-290 ◽  
Author(s):  
MARJORIE B. MEDINA ◽  
ROBERT A. BARFORD ◽  
MARY S. PALUMBO ◽  
LOYD D. ROWE
Keyword(s):  
Bacterial Infections ◽  
High Performance ◽  
Rapid Screening ◽  
Screening Methods ◽  
Detection Range ◽  
Sample Matrix ◽  
Milk Samples ◽  
Immunochemical Detection ◽  
Immunochemical Test ◽  
Layer Chromatography

Sulfamethazine (SMZ) is effective in the treatment of bacterial infections in food producing animals but its use is prohibited in dairy cows. Nevertheless, a 1988 survey of milk in ten cities conducted by the Food and Drug Administration revealed the presence of SMZ. Therefore, it was apparent that there was a need for rapid screening methods for SMZ. We evaluated commercial immunochemical test kits for SMZ with detectabilities of 1–10 parts per billion (ppb). Manipulations are suggested to effectively optimize immunochemical detection of SMZ in raw and processed fluid milk. The performances of the enzyme immunochemical test kits were evaluated by studying the effects of sample preparation, sample matrix, calibration and detection range of the kits using raw and processed milk samples. Immunochemical results were compared to quantitative high performance thin layer chromatography and high performance liquid chromatography with electrochemical detection. Both chromatographic methods had detectabilities in the low parts per billion range.

scholarly journals Application of d-SPE before SPE and HPLC-FLD to Analyze Bisphenols in Human Breast Milk Samples

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4930
Author(s):  
Tomasz Tuzimski ◽  
Szymon Szubartowski
Keyword(s):  
Breast Milk ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Diglycidyl Ether ◽  
Human Breast Milk ◽  
Phase Extraction ◽  
Human Breast ◽  
Milk Samples ◽  
Relative Standard

In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with fluorescence detection (HPLC-FLD) for the simultaneous determination of seven bisphenols (bisphenol F (BPF), bisphenol E (BPE), bisphenol B (BPB), BADGE (bisphenol A diglycidyl ether), BADGE∙2H2O, BADGE∙H2O, BADGE∙2HCl) in human breast milk samples. The dispersive solid phase extraction (d-SPE) coupled with solid phase extraction (SPE) procedure performed well for the majority of the analytes with recoveries in the range 57–88% and relative standard deviations (RSD%) of less than 9.4%. During the d-SPE stage, no significant matrix effect was observed thanks to the application of different pairs of salts such as zirconium-dioxide-based sorbents (Z-Sep or Z-Sep +) and primary secondary amine (PSA) or QuEChERS Enhanced Matrix Removal-Lipid (EMR-Lipid) and PSA. The method limits of quantification (mLOQs) for all investigated analytes were set at satisfactory low values in the range 171.89–235.11 ng mL−1. Analyte concentrations were determined as the average value from human breast milk matrix samples. The results show that the d-SPE/SPE procedure, especially with the application of EMR-Lipid and PSA, could be used for further bisphenol analyses in human breast milk samples.

scholarly journals Six Oligosaccharides’ Variation in Breast Milk: A Study in South China from 0 to 400 Days Postpartum

Nutrients ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 4017
Author(s):  
Shuang Liu ◽  
Xiaokun Cai ◽  
Jin Wang ◽  
Yingyi Mao ◽  
Yan Zou ◽  
...  
Keyword(s):  
Breast Milk ◽  
Early Life ◽  
High Performance ◽  
Anion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Lactating Women ◽  
Time Points ◽  
Milk Samples ◽  
One Year ◽  
High Level

This study investigated the variation in oligosaccharide levels in the breast milk of south Chinese mothers in a prolonged breastfeeding period of up to 400 days postpartum. A total of 488 breast milk samples were collected from 335 healthy mothers at five different time points: 0–5 days, 10–15 days, 40–45 days, 200–240 days, and 300–400 days postpartum. A high-performance anion-exchange chromatography-pulsed amperometric detector (HPAEC-PAD) was used to quantify 2′-fucosyllactose (2′-FL), 3-fucosyllactose (3-FL), lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT), 3′-sialyllactose (3′-SL) and 6′-sialyllactose (6′-SL). In this study, we found six oligosaccharides that were present in breast milk from 0 to 400 days postpartum. The median value ranges of individual oligosaccharide components in this study were 1013–2891 mg/L 2′-FL, 193–1421 mg/L 3-FL, 314–1478 mg/L LNT, 44–255 mg/L LNnT, 111–241 mg/L 3′-SL, and 23–602 mg/L6′-SL. HMO levels decreased over the lactation periods, except for 3-FL, which increased throughout lactation. The predominant fucosylated and sialylated HMOs were 2′-FL and 6′-SL at 40–45 days postpartum and changed to 3-FL and 3′-SL at 200–240 days postpartum. Results from this study showed that lactating women continue to provide their offspring with a high level of 2′-FL one year after delivery, suggesting that 2′-FL may play an important role for infants in early life. Our findings also provide further evidence in support of breastfeeding after one-year postpartum.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

Sign in / Sign up

Export Citation Format

Share Document