A fast and simple LC-ESI-MS/MS method for detecting pyrrolizidine alkaloids in honey with full validation and measurement uncertainty

Valese, Andressa Camargo; Molognoni, Luciano; Ploêncio, Leandro Antunes de Sá; Lima, Flávia Gontijo de; Gonzaga, Luciano Valdemiro; Górniak, Silvana Lima; Daguer, Heitor; Barreto, Fabiano; Costa, Ana Carolina Oliveira

doi:10.1016/j.foodcont.2016.02.050

Cited by 62 publications

(30 citation statements)

References 46 publications

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“…Despite the recognized toxic effect of PAs and reported cases of human and animal poisoning, no maximum residue limits in food and feed have been established (Valese et al 2016). Some European countries such as Germany, Austria, and the Netherlands have introduced acceptable tolerance levels for herbal preparations and extracts.…”

Section: Introductionmentioning

confidence: 99%

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Determination of Pyrrolizidine Alkaloids in Honey with Sensitive Gas Chromatography-Mass Spectrometry Method

2017

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Pyrrolizidine alkaloids (PAs) are secondary metabolites produced by plants as a chemical defense against herbivores. Plants containing PAs are widely distributed in almost all geographical regions posing a risk of honey contamination. To provide safety of honey and decrease the potential risk for the consumers, a sensitive method based on gas chromatography-mass spectrometry enabling determination of a content of 1,2-unsaturated PAs in honey was developed. Honey samples were purified on MCX cartridges, and PAs were eluted with a solvent mixture consisting of ethyl acetate, methanol, ammonia, and triethylamine. Subsequently, 1,2-unsaturated alkaloids were reduced to their common backbone structures and derivatized with heptafluorobutyric anhydride. The method was validated according to SANTE 2015. All received parameters are in consistence with the document requirements as recovery ranged from 73.1 to 93.6%. The repeatability and reproducibility were calculated as relative standard deviation and ranged from 3.9 to 8.6% and from 10.6 to 17.8%, respectively. The limit of quantification was determined as 1 μg kg −1. Good linearity of the method was obtained with the coefficient of determination R 2 > 0.99. The method was applied to 40 Polish and 14 Asian honey sample analyses.

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Section: Introductionmentioning

confidence: 99%

“…Around 40% of Europe's consumption needs are met through honey imports (CBI 2017). As it was revealed, the honey of Central and South America or Australia can contain high rates of PA positive samples with high individual PA levels (EFSA 2011;Dübecke et al 2011;Griffin et al 2015a;Valese et al 2016).…”

Section: Introductionmentioning

confidence: 99%

Determination of Pyrrolizidine Alkaloids in Honey with Sensitive Gas Chromatography-Mass Spectrometry Method

2017

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“…This method is much more sensitive than the Conv‐ICA method. Thus far, the only recent method that has been developed is an LC‐ESI‐MS/MS method that does not require clean‐up steps [limit of quantification (LOQ) of 0.3 ppb in honey samples] . An UPLC‐MS/MS method produced an LOD of 0.4 ppb for MCT determination in feed .…”

Section: Resultsmentioning

confidence: 99%

“…Monocrotaline (MCT) is a toxic compound that belongs to the 1,2‐dehydropyrrolizidine alkaloid (DHPA) group (Figure ). Cereal grains, honey, and herbs are often contaminated with DHPAs, and exposure(s) to these compounds result in various toxicities, including acute hepatitis, gastroenteritis, pulmonary vasculitis and hypertension . In addition, there is evidence from animal models that MCT is carcinogenic upon long‐term exposure .…”

Section: Introductionmentioning

confidence: 99%

Preincubation format for a sensitive immunochromatographic assay for monocrotaline, a toxic pyrrolizidine alkaloid

Yusakul

Sakamoto

Chanpokapaiboon

et al. 2019

Phytochemical Analysis

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Introduction Monocrotaline (MCT), which is classified as a 1,2‐dehydropyrrolizidine alkaloid (DHPA), is a toxic compound that is mainly produced by Crotalaria spp. MCT contamination in cereals and herbs leads to hepatitis, gastroenteritis, pulmonary vasculitis and hypertension, and different types of cancer. The current analytical methods for MCT are complicated and expensive using liquid chromatography equipped with mass spectrometry detection. Objective The aim of this study was to develop a simple and sensitive preincubation format for an immunochromatographic assay (PI‐ICA) for MCT detection. Methodology We conducted the PI‐ICA via incubation of an MCT‐containing sample with an anti‐MCT monoclonal antibody conjugated with colloidal gold before strip dipping. We compared the PI‐ICA detection sensitivity with that of the conventional ICA (Conv‐ICA) format. Results The PI‐ICA was sensitive with a limit of detection (LOD) of 0.61 ng/mL, which is a 16‐fold improvement over the Conv‐ICA format. These results indicated that the PI‐ICA method exhibits high binding specificity for MCT and low cross‐reactivity towards retronecine, retrorsine, senecionine and heliotrine. Sample solutions from plants containing MCT and related DHPAs produced positive results via PI‐ICA analysis. Conclusions The proposed PI‐ICA system provides a highly sensitive method compared to Conv‐ICA. In addition, the developed PI‐ICA method is simple and highly effective for detecting MCT contamination.

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“…Valese et al. investigated method robustness of an LC‐ESI‐MS/MS method for pyrrolizidine alkaloids present in honey samples . Erland et al.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a quality by design enabled robust LC method for estimation of daptomycin in pharmaceutical dosage form

Panda

Bera

Pradhan

2019

Separation Science Plus

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A simple and new validated liquid chromatography method with stability‐indicating potential was established for quantifying daptomycin in formulations using a quality by design approach. Analytical target profile establishment and earmarking critical analytical attributes helped to control the method performance. Further, the control strategies for critical method variables were defined as per method intent. Youden's robustness test was applied with the dual intent of defining control strategies and evaluating method robustness for continuous method improvement. Chromatography for the purpose constituted of methanol: water (pH 3.5 maintained by o‐phosphoric acid), 90:10, v/v as mobile phase flowing at 1.2 mL/min on a C18 column. Photodiode array detector provided the best results at 367 nm. Results for parameters viz. linearity (5‐200 µg/mL), accuracy (> 99%) and precision (< 1%) advocated method reliability. The detection (2.5 µg/mL) and quantitation limits (5 µg/mL) were quite in agreement with method need. In a nutshell, the hyphenation of Youden's test with quality by design approach ensured the development of a reliable chromatography method for routine estimation of daptomycin throughout its product lifecycle.

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A fast and simple LC-ESI-MS/MS method for detecting pyrrolizidine alkaloids in honey with full validation and measurement uncertainty

Cited by 62 publications

References 46 publications

Determination of Pyrrolizidine Alkaloids in Honey with Sensitive Gas Chromatography-Mass Spectrometry Method

Determination of Pyrrolizidine Alkaloids in Honey with Sensitive Gas Chromatography-Mass Spectrometry Method

Preincubation format for a sensitive immunochromatographic assay for monocrotaline, a toxic pyrrolizidine alkaloid

Development and validation of a quality by design enabled robust LC method for estimation of daptomycin in pharmaceutical dosage form

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