Determination of Free Bisphenol A in Commercially Packaged Ready-to-Consume Carbonated/Non-Carbonated and Non-Alcoholic Beverages with Immunoaffinity Column Purification and UPLC with Fluorescence Detector, First Action 2019.07

2020 ◽  
Author(s):  
Jianmin Liu ◽  
Justine Yu ◽  
Danrey Toth ◽  
Jinchuan Yang ◽  
Lingyun Chen
Keyword(s):  
Bisphenol A ◽  
Orange Juice ◽  
Soft Drink ◽  
Performance Criteria ◽  
Alcoholic Beverages ◽  
Immunoaffinity Column ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Alcoholic Drinks

Abstract Background Bisphenol A (BPA) is a chemical of concern in the food industry. There is a need for a sensitive analytical method for the determination of BPA in beverages. Objective To develop a method for the determination of BPA in carbonated, non-carbonated, and non-alcoholic drinks. Method Replicates of a carbonated soft drink, orange juice with pulp, and a dairy-based coffee drink at spiking levels ranging from 0 to 32 ng/mL were analyzed. The carbonated soft drink was adjusted to pH 7.4 and diluted with phosphate buffered saline (PBS). The orange juice with pulp and the dairy-based coffee drink were extracted with methanol and sodium chloride, then diluted with PBS. Results LOD ranged from 0.06 to 0.08 ng/mL and LOQ ranged from 0.10 to 0.14 ng/mL. Recoveries of BPA from all sample types at 1 to 16 ng/mL spiked levels were between 93 and 100%; relative standard deviation (RSDr, %) ranged from 0.71 to 8.38% depending on matrix and spiking levels. Conclusions The results indicate that the method for determination of BPA in carbonated, non-carbonated, and non-alcoholic drinks is reproducible and meets AOAC Official MethodSM performance criteria. Highlights The test portions were filtered and the filtrates applied to an immunoaffinity column (IAC) containing antibodies specific for BPA. After the column was washed with water, BPA was eluted from the IAC with 80% methanol and the eluate was directly injected, or concentrated and injected, into ultra-performance liquid chromatography (UPLC) with fluorescence detector (FLD) for separation, detection, and quantitation.

Determination of Aflatoxins and Ochratoxin A in Traditional Turkish Cereal-Based Fermented Food by Multi-Affinity Column Cleanup and LC Fluorescence Detection: Single-Laboratory Validation

2019 ◽  
Vol 102 (1) ◽  
pp. 156-163 ◽  
Author(s):  
Tugrul Kaymak ◽  
Ercan Koca ◽  
Mustafa Atak ◽  
Ercan Sarikaya ◽  
Joerg Stroka
Keyword(s):  
Ochratoxin A ◽  
Fluorescence Detection ◽  
Performance Criteria ◽  
Immunoaffinity Column ◽  
Method Performance ◽  
Column Method ◽  
Relative Standard ◽  
Varied Composition ◽  
Single Laboratory

Abstract Background: Tarhana is a traditional fermented, sun-dried Turkish food containing yogurt and cereals. There are several potential sources of mycotoxins in tarhana, such as contamination of ingredients or formation during preparation, when water activity is suitable for fungal growth and may lead to mycotoxin production during fermentation or subsequent sun-drying. Objective: To optimize an immunoaffinity column method and carry out single-laboratory validation for the determination of aflatoxins B1, B2, G1, and G2 together with ochratoxin A (OTA) in tarhana. Method: A homogenized sample was extracted with methanol–acetonitrile–water (25 + 25 + 50) using a high-speed blender. The sample extract was filtered, diluted with phosphate buffered saline (PBS) solution, and applied to a multi-immunoaffinity column (AFLAOCHRA PREP®). Aflatoxins and OTA were removed with neat methanol and then directly analyzed by reverse-phase LC with fluorescence detection using post-column bromination (Kobra® Cell). Results: Test portions of blank tarhana were spiked with a mixture of total aflatoxins and OTA to give levels ranging from 2.5 to 10.0 and 1.5 to 6.0 μg/kg, respectively. Recoveries for total aflatoxins and OTA ranged from 82 to 93 and 78 to 94%, respectively, for spiked samples. Based on results for spiked tarhana (30 replicates, each at three levels), the relative standard deviation for repeatability ranged from 1.4 to 7.2 and 3.6 to 7.7% for total aflatoxins and OTA, respectively. Conclusions: The performance characteristics for recovery, repeatability, and sensitivity have demonstrated that the method meets method performance criteria for use for official purposes. The method was demonstrated as being applicable to naturally contaminated samples of tarhana of varied composition obtained from local markets in Turkey. Highlights: This is the first immunoaffinity column method for simultaneous analysis of aflatoxins and OTA in traditional Turkish food (tarhana). Suitability was demonstrated by single-laboratory validation for official purposes in Turkey. The method was demonstrated as suitable for naturally contaminated samples of tarhana of varied composition.

scholarly journals Combination of the QuEChERS with the Dispersive Liquid-liquid Microextraction and Derivatisation in the Determination Diethylstilbestrol and Bisphenol A in Products by Gas-liquid Chromatography

2012 ◽  
Vol 12 (4) ◽  
pp. 17-22
Author(s):  
V. G. Amelin ◽  
◽  
D. S. Korolev ◽  
A. V. Tretyakov ◽  
◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Bisphenol A ◽  
Alcoholic Beverages ◽  
Gas Liquid Chromatography ◽  
Rapid Procedure ◽  
Relative Standard ◽  
Canned Foods ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A simple and rapid procedure of simultaneous determination of diethylstilbestrol and bisphenol A in canned foods (1–250 and 0.5–125 µg kg-1, respectively), drinking water, alcoholic and no alcoholic beverages (0.25-50 µg L-1 and 0.1–25 µg L-1, respectively) by gas-liquid chromatography with a detector to capture electrons developed. Diethylstilbestrol and bisphenol A from food was extracted with acetonitrile by the method of QuEChERS. Further purification and concentration of the extract was carried dispersive liquid-liquid microextraction carbon tetrachloride. The duration of the analysis was 1–1.5 h, the relative standard deviation of the results of analysis does not exceed 0.1.

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

scholarly journals Determination of Ochratoxin A in Wine and Beer by Immunoaffinity Column Cleanup and Liquid Chromatographic Analysis with Fluorometric Detection: Collaborative Study

2001 ◽  
Vol 84 (6) ◽  
pp. 1818-1827 ◽  
Author(s):  
Angelo Visconti ◽  
Michelangelo Pascale ◽  
Gianluca Centonze ◽  
E Anklam ◽  
A M Betbeder ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Red Wine ◽  
Collaborative Study ◽  
White Wine ◽  
Fluorometric Detection ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

scholarly journals Immunoaffinity Column Cleanup with Liquid Chromatography Using Post-Column Bromination for Determination of Aflatoxins in Hazelnut Paste: Interlaboratory Study

2005 ◽  
Vol 88 (2) ◽  
pp. 526-535 ◽  
Author(s):  
Hamide Z Senyuva ◽  
John Gilbert
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Aflatoxin B1 ◽  
The United States ◽  
Interlaboratory Study ◽  
Immunoaffinity Column ◽  
Test Portion ◽  
Relative Standard

Abstract An interlaboratory study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for determination of aflatoxin B1 and total aflatoxins in hazelnut paste at European regulatory limits. The test portion was extracted with methanol–water (6 + 4). The extract was filtered, diluted with phosphate-buffered saline (PBS) solution to a specified solvent concentration, and applied to an immunoaffinity column containing antibodies specific to aflatoxins. The aflatoxins were removed from the immunoaffinity column with methanol, and then quantified by reversed-phase LC with post-column derivatization (PCD) involving bromination. The PCD was achieved with electrochemically generated bromine (Kobra Cell®) followed by fluorescence detection (except for one participant who used pyridinum hydrobromide perbromide for bromination). Hazelnut paste, both naturally contaminated with aflatoxins and blank (<0.1 ng/g) for spiking by participants with aflatoxins, was sent to 14 collaborators in Belgium, The Netherlands, Spain, Turkey, the United Kingdom, and the United States. Test portions were spiked at levels of 4.0 and 10.0 ng/g for total aflatoxins by participants using supplied total aflatoxins standards. Recoveries for total aflatoxins and aflatoxin B1 averaged from 86 to 89%. Based on results for naturally contaminated samples (blind duplicates at 3 levels ranging from 4.0 to 11.8 ng/g total aflatoxins), the relative standard deviation for repeatability (RSDr) ranged from 2.3 to 3.4% for total aflatoxins and from 2.2 to 3.2% for aflatoxin B1. The relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 7.0% for total aflatoxins and from 7.3 to 7.8% for aflatoxin B1. The method showed exceptionally good within-laboratory and between-laboratory precision for hazelnut paste, as evidenced by HORRAT values, which in all cases were significantly below target levels, the low levels of determination for both aflatoxin B1 and total aflatoxins.

scholarly journals Multiresidue Determination of Fluoroquinolones in Shrimp by Liquid Chromatography-Fluorescence-Mass Spectrometryn

2005 ◽  
Vol 88 (4) ◽  
pp. 1160-1166 ◽  
Author(s):  
Marilyn J Schneider ◽  
Luz Vazquez-Moreno ◽  
Maria del Carmen Bermudez-Almada ◽  
Ramon Barraza Guardado ◽  
Magdalena Ortega-Nieblas
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Phosphate Buffer ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Product Ions ◽  
Multiresidue Determination ◽  
Shrimp Tissue

Abstract An efficient multiresidue method for analysis of fluoroquinolones in shrimp has been developed in which quantitation by fluorescence and confirmation by Multiple Stage Mass Spectrometry (MSn) is achieved simultaneously. In this method, shrimp tissue is extracted with ammoniacal acetonitrile and the extract is defatted and then evaporated. After dissolution in basic phosphate buffer, fluoroquinolones in the extract are separated by liquid chromatography and quantitated, taking advantage of their intense fluorescence. Eluate from the fluorescence detector enters the MSn, which allows for confirmation by monitoring ratios of 2 prominent product ions in the MS3 or MS2 spectrum. Using this method, 8 fluoroquinolones have been analyzed in shrimp samples fortified at 10, 25, 50, or 100 ppb levels. Recoveries for desethyleneciprofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin ranged from 75 to 92%, with relative standard deviation values of <6%. The limits of quantitation ranged from 0.1 to 1 ng/g. Enrofloxacin and ciprofloxacin were also successfully determined in enrofloxacin-incurred shrimp using this method.

Spectrophotometric Determination of Cyclamate in Soft Drinks and Desserts: Complementary Collaborative Study

1988 ◽  
Vol 71 (6) ◽  
pp. 1212-1214
Author(s):  
Anna-Maija K SJÖBERG
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Soft Drink ◽  
Collaborative Study ◽  
Soft Drinks ◽  
Food Control ◽  
Average Recovery ◽  
Relative Standard ◽  
Standard Deviations

Abstract Fifteen official food control laboratories participated in a collaborative study of a spectrophotometric method to determine cyclamate in a soft drink and a dessert at concentrations of 90-311 mg/L and 202-526 mg/kg, respectively, with blind duplicates and a blank. Average recovery from the soft drink was 97.5%, and from the dessert, 98.6%. Reproducibility relative standard deviations were 4.7-6.5% and 6.9-8.5%, respectively. The outlier percentage was 5.5%. This study complements an earlier work by leading Nordic food laboratories and was designed according to the latest recommendations. The results of this study were compared with those of the earlier collaborative study and with general collaborative results obtained by AOAC.

scholarly journals Determination of Naringin and Neohesperidin in Orange Juice by Liquid Chromatography with UV Detection to Detect the Presence of Grapefruit Juice: Collaborative Study

2000 ◽  
Vol 83 (5) ◽  
pp. 1155-1166 ◽  
Author(s):  
Wilbur Widmer ◽  
A Brause ◽  
E Coppola ◽  
K Daniels ◽  
R Feicht ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Orange Juice ◽  
Sodium Benzoate ◽  
Grapefruit Juice ◽  
Collaborative Study ◽  
Potassium Sorbate ◽  
Sour Orange ◽  
Relative Standard ◽  
Standard Deviations

Abstract Fifteen collaborating laboratories were sent 9 samples of citrus juice mixtures as blind duplicates for determination of naringin and neohesperidin by liquid chromatography. Two sample pairs were 100% orange juice and did not contain any naringin or neohesperidin. The remaining 7 sample pairs contained naringin at levels ranging from 3.9 to 46.5 ppm and neohesperidin at levels ranging from 0.14 to 35.6 ppm. Five sample pairs consisted of orange juice mixtures containing 1, 3, and 5% grapefruit juice; 5% sour orange; and 5% K-Early citrus variety. Two sample pairs were orange juice spiked with naringin, neohesperidin, sodium benzoate, and potassium sorbate. Data were received from 13 laboratories. Data from 1 collaborator were eliminated because the method protocol was not followed. Neohesperidin values from another laboratory were also not used because of problems with a coeluting component. Repeatability relative standard deviations ranged from 2.95 to 15.23% for naringin and from 3.00 to 11.74% for neohesperidin. Reproducibility relative standard deviations ranged from 11.34 to 31.94% for naringin and from 10.45 to 26.17% for neohesperidin. The method is reliable for detecting the presence of grapefruit juice in orange juice as indicated by a finding of ≥10 ppm naringin and ≤2 ppm neohesperidin. The method was adopted First Action by AOAC INTERNATIONAL.

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