Current Perspectives and Recommendations for the Development of Mass Spectrometry Methods for the Determination of Allergens in Foods

Abstract Allergen detection and quantification is an essential part of allergen management as practiced by food manufacturers. Recently, protein MS methods (in particular, multiple reaction monitoring experiments) have begun to be adopted by the allergen detection community to provide an alternative technique to ELISA and PCR methods. MS analysis of proteins in foods provides additional challenges to the analyst, both in terms of experimental design and methodology: (1) choice of analyte, including multiplexing to simultaneously detect several biologically relevant molecules able to trigger allergic reactions; (2) choice of processing stable peptide markers for different target analytes that should be placed in publicly available databases; (3) markers allowing quantification (e.g., through standard addition or isotopically labeled peptide standards); (4) optimization of protease digestion protocols to ensure reproducible and robust method development; and (5) effective validation of methods and harmonization of results through the use of naturally incurred reference materials spanning several types of food matrix.

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NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2016v8i9.11968 ◽

2016 ◽

Vol 8 (9) ◽

pp. 61 ◽

Cited By ~ 6

Author(s):

Narottam Pal ◽

Avanapu Srinivasa Rao ◽

Pigilli Ravikumar

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Human Plasma ◽

Method Development ◽

Multiple Reaction Monitoring ◽

Internal Standard ◽

New Method ◽

Liquid Chromatography Mass Spectrometry ◽

Chromatography Mass Spectrometry

Objective: To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).Methods: The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C8, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.Results: The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.Conclusion: Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.

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SENSITIVE BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF VENETOCLAX IN HUMAN PLASMA BY LC-ESI-MS/MS

INDIAN DRUGS ◽

10.53879/id.57.06.11999 ◽

2020 ◽

Vol 57 (06) ◽

pp. 32-38

Author(s):

H. Potluri ◽

Keyword(s):

Human Plasma ◽

Method Development ◽

Multiple Reaction Monitoring ◽

Internal Standard ◽

Liquid Liquid Extraction ◽

Liquid Chromatography Tandem Mass ◽

Positive Mode ◽

Method Development And Validation ◽

Development And Validation

A specific and sensitive method of liquid chromatography–tandem mass spectrometry was demonstrated for the experimental determination of venetoclax in human plasma utilising venetoclax-D8 as an internal standard. The column Xbridge C18, 50 × 4.6mm, 5 µm was used for attaining chromatographic separation by utilising 10mM ammonium formate and methanol as isocratic mobile phase in the composition ratio of 20:80 (V/V). The flow-rate selected was 0.7ml/min. Venetoclax and venetoclax-D8 are identified in multiple reaction monitoring (MRM) positive mode with proton adducts at m/z 869.53 →553.21 and m/z 877.14 → 553.23, respectively. For the successful extraction of drug as well as internal standard, liquid-liquid extraction technique was efficiently utilised. The developed technique was established in a linear concentration range of 5.0-5000.0 pg/ml along with correlation coefficient (r2) of 0.9994. Intra and inter-day precisions were found to be 0.7 to 1.90% and 0.7 to 2.0 % for venetoclax and venetoclax-D8, respectively. Accuracy was found to be within 98.6 to 101.99% and 99.17 to 101.14 % for venetoclax and venetoclax-D8, respectively. It was observed that throughout the bench top studies, post-operative stability studies and freeze-thawing cycles, venetoclax retained stability.

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Determination of Iron (Fe) and Calcium (Ca) in NIST SRM 1566b (Oyster tissue) using Flame Atomic Absorption Spectrometry (F-AAS) by Standard Addition Method

Jurnal Kimia VALENSI ◽

10.15408/jkv.v2i2.205 ◽

2011 ◽

Vol 2 (2) ◽

Author(s):

Fitri Dara ◽

Y Susanto Ridwan

Keyword(s):

Atomic Absorption Spectrometry ◽

Atomic Absorption ◽

Flame Atomic Absorption Spectrometry ◽

Inductively Couple Plasma ◽

Standard Addition ◽

Absorption Spectrometry ◽

Oyster Tissue ◽

Food Matrix ◽

Flame Atomic Absorption

NIST Standard Reference Material (SRM 1566b) was employed for the determination of Iron (Fe) andCalcium (Ca) as nutrients in food matrix using Flame Atomic Absorption Spectrometry (F-AAS). Thecertified value of SRM 1566b for Fe and Ca are 205.8 ± 6.8 mg/kg and 0.0838 ± 0.0020 (%) or 838 ±20 mg/kg, respectively. This certified values are based on results obtained by single primary method(Isotope Dilution Inductively Couple Plasma Mass Spectrometry) at NIST with confirmation by othermethods at National Metrology Institute of P.R. China. This paper proposed a method fordetermination of Fe and Ca in food matrix as recommended by AOAC official with a littlemodification. The method was commenced from the destruction of all organic matter by dry oxidationbefore analysis by standard addition. Under optimum condition, the results of the determination of Feand Ca in SRM 1566b were agreed well with the certificate value. This method would be useful forroutine analysis in food testing laboratories.

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New LC-MS Method Development and Validation for Quantitative Estimation of 2-Acetoxy Ethyl Acetoxy Methyl Ether in Acyclovir

Research Journal of Pharmacy and Technology ◽

10.52711/0974-360x.2021.01022 ◽

2021 ◽

pp. 5881-5885

Author(s):

Indhu Priya Mabbu ◽

G. Sumathi ◽

N. Devanna

Keyword(s):

Methyl Ether ◽

Method Development ◽

Quantitative Estimation ◽

Signal To Noise Ratio ◽

Multiple Reaction Monitoring ◽

Ratio Method ◽

Triple Quadrupole Mass Spectrometer ◽

Method Development And Validation ◽

Development And Validation

The objective of the proposed method is to develop and validate a specific, precise and accurate LC-MS method for the determination of 2-acetoxy ethyl acetoxy methyl ether (AEM) in Acyclovir. An isocratic separation was done by using YMC-PACK PRO C18, (150 x 4.6 mm, 3µm) column with a mobile phase composition of Buffer (0.1% Ammonia in water) : Methanol(25 :75v/v)at a flow rate of 0.4mL/min, diluent solution of 0.2% of 0.1N NaOH in Methanol were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) Acquisition mode and possitive polarity mode. The Retention time of AEM was found to be 5.344 minutes, LOD and LOQ were observed at 0.03 ppm and 0.11 ppm concentration respectively by signal to noise ratio method, linearity was found in the concentration range of 0.18-0.55 ppm with correlation coefficient of 0.996 and accuracy in the range of 97.7- 101% was obtained by performing percentage recovery studies. The % RSD was observed to be less than 10% for six replicates said to be precise. The proposed method was validated for accuracy, precision, sensitivity, and linearity successfully employed for quantitative determination of AEM in acyclovir.

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Simultaneous Determination of Methamphetamine and Its Isomer N-Isopropylbenzylamine in Forensic Samples by Using a Modified LC-ESI-MS/MS Method

Journal of Nanomaterials ◽

10.1155/2021/6679515 ◽

2021 ◽

Vol 2021 ◽

pp. 1-9

Author(s):

Yangxu Luo ◽

Juan Du ◽

Huadi Xiao ◽

Ling Zheng ◽

Xuncai Chen ◽

...

Keyword(s):

Simultaneous Determination ◽

Limit Of Detection ◽

Multiple Reaction Monitoring ◽

Acetate Solution ◽

Accurate Identification ◽

Esi Ms ◽

Target Analytes ◽

Relative Standard ◽

Forensic Samples

Accurate identification and quantification of methamphetamine (MA) and its related substances are essential for the investigation and fair trial of drug offenses. In this study, a modified LC-ESI-MS/MS method for the simultaneous determination of MA and its isomer N-isopropylbenzylamine (N-IBA) in forensic samples was developed and validated. Optimum chromatographic separation of the target analytes was achieved on an Agilent Poroshell 120 SB-C18 column ( 4.6 × 100 mm, 2.7 μm) at 40°C with isocratic elution at the flow rate of 0.40 mL/min. The mobile phase was acetonitrile and 20 mM ammonium acetate solution containing 0.1% formic acid (80 : 20, v / v ). Positive ESI-MS/MS detection was performed in multiple reaction monitoring (MRM) mode to identify and quantify the target analytes. Method validation showed excellent linearity in the range of 0.51 ng/mL~51 ng/mL for MA and N-IBA. The low limit of detection (LLOD) and low limit of quantification (LLOQ) reached 0.1 ng/mL and 0.3 ng/mL for both analytes. The method showed a satisfactory accuracy with an inter- and intraday-relative error (RE) <20%, and a precision of inter- and intraday relative standard deviation (RSD) less than 15%. The validated method was successfully applied in real forensic samples and resulted in the detection of MA and N-IBA in 8 suspected samples in drug cases that only deemed MA positive using our previous routine screening procedure, which avoided the misidentification of N-IBA as MA.

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An accurate and sensitive effervescence-assisted liquid phase microextraction method for the determination of cobalt after a Schiff base complexation by slotted quartz tube-flame atomic absorption spectrophotometry in urine samples

Analytical Methods ◽

10.1039/d0ay02264k ◽

2021 ◽

Author(s):

Tülay Borahan ◽

Buse Zaman ◽

Büşra Sümeyye Arıca Polat ◽

Gülhan Bakırdere ◽

Sezgin Bakırdere

Keyword(s):

Method Development ◽

Atomic Absorption Spectrophotometry ◽

Urine Samples ◽

Flame Atomic Absorption Spectrophotometry ◽

Liquid Phase Microextraction ◽

Absorption Spectrophotometry ◽

Flame Atomic Absorption ◽

Target Analytes ◽

Slotted Quartz Tube

In this study, an accurate analytical method development for cobalt determination in urine samples was described. The method is based on the mass transfer of the target analytes to the...

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