Perspective on Advancing FDA Regulatory Monitoring for Mycotoxins in Foods using Liquid Chromatography and Mass Spectrometry (Review)

2016 ◽  
Vol 99 (4) ◽  
pp. 890-894 ◽  
Author(s):  
Kai Zhang ◽  
Jon W Wong ◽  
Alexander J Krynitsky ◽  
Mary W Trucksess
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Food Safety ◽  
High Resolution ◽  
Drug Administration ◽  
Matrix Effects ◽  
Tandem Ms ◽  
Mycotoxin Analysis ◽  
Lc Tandem Ms ◽  
The U.S

Abstract The presence of mycotoxins (such as aflatoxins, deoxynivalenol, fumonisins, and patulin) is routinely monitored by the U.S. Food and Drug Administration (FDA) to ensure that their concentrations in food are below the levels requiring regulatory action or advisories. To improve the efficiency of mycotoxin analysis, the researchers at the FDA's Center for Food Safety and Applied Nutrition have been evaluating modern LC-MS technologies. Consequently, a variety of LC–tandem MS and LC–high-resolution MS methods have been developed, which simultaneously identify and quantitate multiple mycotoxins in foods and feeds. Although matrix effects (matrix-induced ion suppression or enhancement) associated with LC-MS-based mycotoxin analysis remain, this review discusses methods for managing these effects and proposes practical solutions for the future implementation of LC-MS-based multimycotoxin analysis.

The evaluation of matrix effects in pesticide multi-residue methods via matrix fingerprinting using liquid chromatography electrospray high-resolution mass spectrometry

2016 ◽  
Vol 8 (23) ◽  
pp. 4664-4673 ◽  
Author(s):  
María del Mar Gómez-Ramos ◽  
Łukasz Rajski ◽  
Ana Lozano ◽  
Amadeo R. Fernández-Alba
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Matrix Effects ◽  
High Resolution Mass Spectrometry ◽  
High Resolution Mass ◽  
P Matrix ◽  
Resolution Mass

Matrix fingerprinting of twenty-three different commodities was evaluated.

scholarly journals Pilot Study for the Standardization of Insulin Immunoassays with Isotope Dilution–Liquid Chromatography/Tandem Mass Spectrometry

2007 ◽  
Vol 53 (8) ◽  
pp. 1462-1469 ◽  
Author(s):  
Diego Rodríguez-Cabaleiro ◽  
Katleen Van Uytfanghe ◽  
Veronique Stove ◽  
Tom Fiers ◽  
Linda M Thienpont
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Pilot Study ◽  
Total Error ◽  
Method Comparison ◽  
Tandem Ms ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Lc Tandem Ms

Abstract Background: An international working group convened by the American Diabetes Association (ADA) called for a reference measurement procedure for use in a trueness-based standardization project of insulin immunoassays. In view of this demand, we conducted a pilot study to investigate the feasibility of such a standardization project with our isotope dilution-liquid chromatography/tandem mass spectrometry (ID-LC/tandem MS) procedure. Methods: We evaluated the precision, accuracy, and limit of quantification (LoQ) of the ID-LC/tandem MS procedure by use of insulin-free serum supplemented with insulin to give 3 pools with concentrations of 0.0796, 0.769, and 5.56 μg/L. We conducted a pilot method comparison study with 4 immunoassays and 80 samples from fasting and glucose-stimulated patients. Results: The within-run and total imprecision (CV) ranged from 3.2% to 6.3% and from 4.9% to 12.1% (listing sequence from the high to the low pool). The recovery from supplemented insulin-free sera ranged from 101.8% to 104.1%, and the LoQ was 0.07 μg/L (12 pmol/L). Weighted Deming regression and correlation analysis of the method-comparison data showed considerable between-assay variation for the immunoassays but, with the exception of one assay, excellent correlation with ID-LC/tandem MS. Recalibration of the immunoassay results considerably reduced the between-assay variation. Moreover, after recalibration, 3 of the 4 assays fulfilled the total error specification of 32% proposed by the ADA Workgroup. Conclusions: Recalibration of insulin assays by regression equations established from method comparison with ID-LC/tandem MS can result in successful standardization and fulfillment of the total error criterion proposed by the ADA Workgroup.

scholarly journals Evaluation of Different Tandem MS Acquisition Modes to Support Metabolite Annotation in Human Plasma Using Ultra High-Performance Liquid Chromatography High-Resolution Mass Spectrometry for Untargeted Metabolomics

Metabolites ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 464
Author(s):  
Julian Pezzatti ◽  
Víctor González-Ruiz ◽  
Julien Boccard ◽  
Davy Guillarme ◽  
Serge Rudaz
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Human Plasma ◽  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
Tandem Ms ◽  
Metabolite Annotation ◽  
Resolution Mass

Ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) is a powerful and essential technique for metabolite annotation in untargeted metabolomic applications. The aim of this study was to evaluate the performance of diverse tandem MS (MS/MS) acquisition modes, i.e., all ion fragmentation (AIF) and data-dependent analysis (DDA), with and without ion mobility spectrometry (IM), to annotate metabolites in human plasma. The influence of the LC separation was also evaluated by comparing the performance of MS/MS acquisition in combination with three complementary chromatographic separation modes: reversed-phase chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) with either an amide (aHILIC) or a zwitterionic (zHILIC) stationary phase. RPLC conditions were first chosen to investigate all the tandem MS modes, and we found out that DDA did not provide a significant additional amount of chemical coverage and that cleaner MS/MS spectra can be obtained by performing AIF acquisitions in combination with IM. Finally, we were able to annotate 338 unique metabolites and demonstrated that zHILIC was a powerful complementary approach to both the RPLC and aHILIC chromatographic modes. Moreover, a better analytical throughput was reached for an almost negligible loss of metabolite coverage when IM-AIF and AIF using ramped instead of fixed collision energies were used.

scholarly journals Detection of Methylphenidate in Equine Hair Using Liquid Chromatography–High-Resolution Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5798
Author(s):  
Benjamin C. Moeller ◽  
Luis Flores ◽  
Amel Clifford ◽  
Gwendolyne Alarcio ◽  
Mary Mosburg ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Matrix Effects ◽  
High Resolution Mass Spectrometry ◽  
Horse Racing ◽  
High Resolution Mass ◽  
Accuracy And Precision ◽  
Product Ions ◽  
Resolution Mass

Methylphenidate is a powerful central nervous system stimulant with a high potential for abuse in horse racing. The detection of methylphenidate use is of interest to horse racing authorities for both prior to and during competition. The use of hair as an alternative sampling matrix for equine anti-doping has increased as the number of detectable compounds has expanded. Our laboratory developed a liquid chromatography–high-resolution mass spectrometry method to detect the presence of methylphenidate in submitted samples. Briefly, hair was decontaminated, cut, and pulverized prior to liquid–liquid extraction in basic conditions before introduction to the LC-MS system. Instrumental analysis was conducted using a Thermo Q Exactive mass spectrometer using parallel reaction monitoring using a stepped collision energy to obtain sufficient product ions for qualitative identification. The method was validated and limits of quantitation, linearity, matrix effects, recovery, accuracy, and precision were determined. The method has been applied to confirm the presence of methylphenidate in official samples submitted by racing authorities.

scholarly journals Feasibility of Standardization of Serum C-Peptide Immunoassays with Isotope-Dilution Liquid Chromatography–Tandem Mass Spectrometry

2006 ◽  
Vol 52 (6) ◽  
pp. 1193-1196 ◽  
Author(s):  
Diego Rodríguez Cabaleiro ◽  
Dietmar Stöckl ◽  
Jean M Kaufman ◽  
Tom Fiers ◽  
Linda M Thienpont
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Isotope Dilution ◽  
Method Comparison ◽  
Measurement Procedure ◽  
Tandem Ms ◽  
C Peptide ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
Lc Tandem Ms

Abstract Background: Serum C-peptide concentrations reflect pancreatic function in different clinical and diagnostic settings; however, the utility of C-peptide testing is limited by the lack of standardized commercial immunoassays. Standardization can best be done by split-sample comparison with a hierarchically higher reference measurement procedure with a set of native sera. For serum peptides, isotope-dilution liquid chromatography–mass spectrometry (ID-LC/MS) is recommended as a reference measurement procedure. Methods: We evaluated the analytical performance characteristics of an ID-LC/tandem MS procedure for measurement of serum C-peptide after a 2-step solid-phase extraction. To investigate the feasibility of this procedure for use in standardization, we also performed a method comparison with 3 representative commercial assays. Results: The ID-LC/tandem MS procedure showed maximum within-run, between-run, and total CVs on dedicated sera (C-peptide concentrations, 1.6 and 4.0 μg/L) of 2.1%, 2.5%, and 2.9%, respectively; an accuracy of 94.6%–104.1%; a minimum trueness of 98.1% (95% confidence interval, 96.2%–100.0%), and limits of quantification and detection of 0.15 and 0.03 μg/L, respectively. Deming linear regression analysis of the method-comparison data showed that the immunoassays correlated well with ID-MS and were specific, but lacked intercomparability and trueness. We propose that the deficiencies can be resolved by recalibration on the basis of the method comparison. Conclusions: The ID-LC/tandem MS procedure is suitable for specific and accurate measurement of basal and stimulated serum concentrations of proinsulin C-peptide fragment 33–63 and is suitable for use in standardization of C-peptide immunoassays.

A High-Resolution Liquid Chromatography-Mass Spectrometry Method for Identification of Toxic Natural Products in Clinical Cases

2020 ◽  
Vol 154 (Supplement_1) ◽  
pp. S128-S128
Author(s):  
Y R Luo ◽  
C Yun ◽  
K L Lynch ◽  
K Comstock
Keyword(s):  
Mass Spectrometry ◽  
Natural Products ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Mass Spectrometer ◽  
Matrix Effects ◽  
Urine Samples ◽  
Spectral Library ◽  
Serum Samples ◽  
Clinical Cases

Abstract Introduction/Objective Many natural products have biological effects on humans and animals. Poisoning caused by natural products is often found in clinical toxicology cases. Liquid chromatography-high-resolution-mass spectrometry (LC-HRMS) has recently emerged as a powerful analytical tool for large-scale target screening, and the application of LC-HRMS can be expanded to solve the clinical cases of natural product poisoning. Methods The LC-HRMS method is based on a spectral library of 121 natural products. The spectral library was constructed by analyzing standards either in a Q-TOF mass spectrometer (only MS2 spectra acquired) or in an Orbitrap Tribrid mass spectrometer (MS2 and MS3 spectra acquired). Results The LC-HRMS method was verified for the limit of detection (LOD) and matrix effects in both serum and urine matrices. For each compound, the LOD was evaluated from 1.0 ng/ml to 1000 ng/ml for urine samples and from 0.50 ng/ml to 500 ng/ml for serum samples. The matrix effects were determined at three concentration levels andranged from 30.4% to 123.5% for urine samples and from 23.4% to 132.9% for serum samples. The LC-HRMS method was successfully applied to identify the culprits in three clinical cases. In addition, the combined use of MS2 and MS3 spectra enhanced the accuracy of compound identification, in library search reducing the importance of retention time that varies among instruments and consumable lots. In Case 1, the patient presented with paresthesias, arrhythmias, and stiffened arms and legs. The toxic alkaloid aconitine was identified in the serum sample and the extract of herbs that the patient ingested. In Case 2, the patients presented with weakness, dizziness, and vomiting. The symptoms were caused by mistakenly taking Nicotiana glauca leaves and the alkaloid anabasine was identified as the culprit. In Case 3, the patients were suspected of intoxicated by taking too much extract of lupini beans. The culprit alkaloids from lupini beans lupanine and sparteine were found in the serum samples. Conclusion The involvement of a toxicology laboratory with the capability to perform the LC-HRMS method and with experience in the investigation of undifferentiated cases provides a unique diagnostic advantage in cases where exposure to toxic substances is possible.

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