Validation Study of Histamine Test for the Determination of Histamine in Selected Fish Products

2019 ◽  
Vol 102 (1) ◽  
pp. 164-180 ◽  
Author(s):  
Kazuhiko Shimoji ◽  
Mikio Bakke ◽  
James M Hungerford ◽  
Christina A Mireles DeWitt ◽  
Sevim Köse
Keyword(s):  
Biogenic Amines ◽  
Validation Study ◽  
Optical Path Length ◽  
Cross Reactivity ◽  
Assay Method ◽  
Fish Sauce ◽  
Canned Tuna ◽  
Reactivity Test ◽  
Regulatory Bodies

Abstract Background: Since prescribed limits for histamine in fish have been set by various regulatory bodies around the world, the rapid, specific and easy determination of histamine is in high demand. Objective: The enzymatic histamine assay developed by Kikkoman Biochemifa Co. was validated. Methods: Fresh and frozen raw tuna, canned tuna in oil and water, and anchovy fish sauce were used for the validation study under the specific guidelines of the AOAC Research Institute Performance Tested MethodSM (PTM) program. Results: Good linearity (R2 > 0.9997) for histamine standard solutions, recovery rates (90.3–125.2%), and repeatability precisions (RSDr < 10%) were shown for all spiked tested matrixes. The claimed LOQ values, 20 and 10 mg/kg for solid fish and 160 and 80 mg/kg for fish sauce using a 1 and 2 cm optical path length spectrophotometer, respectively, were validated. The cross-reactivity test showed no positive interference of other biogenic amines, except for agmatine and putrescine. Moreover, no inhibition was confirmed among the 12 biogenic amines. Stability data supported the shelf life (42 months at 4°C), lot-to-lot consistency was demonstrated, and the method was shown to be robust. Independent laboratory testing using canned tuna in oil demonstrated that the recovery ranged from 93.5 to 124.7%, and the RSDr at all spike levels was <20%. Conclusions: The simple and rapid enzymatic histamine assay method has been successfully validated. Highlights: This histamine quantitative assay kit was qualified for PTM certification No. 041802.

scholarly journals Validation Study of MaxSignal® Histamine Enzymatic Assay for the Detection of Histamine in Fish/Seafood

2018 ◽  
Vol 101 (3) ◽  
pp. 783-792 ◽  
Author(s):  
Swapna Gone ◽  
Nicolas Kosa ◽  
Joseph Krebs ◽  
James Hungerford ◽  
Mary Trucksess ◽  
...  
Keyword(s):  
Biogenic Amines ◽  
Validation Study ◽  
Background Level ◽  
Cross Reactivity ◽  
Study Data ◽  
Stability Study ◽  
Enzymatic Assay ◽  
Assay Method ◽  
Canned Tuna ◽  
Fresh Frozen

Abstract Bioo Scientific Corp. has developed a rapid enzymatic quantitative assay for the determination of histamine in seafood. Fresh/frozen tuna, canned tuna, pouched tuna, and frozen mahi mahi samples were used for the validation study under the specific guidelines of the AOAC Research Institute Performance Tested MethodsSM program. Recoveries ranged from 82 to 107% at concentrations ranging from 6 to 72 ppm, with RSDr values between 0.8 and 6.5% (6–72 ppm). The linearity of the assay ranged from 0 to 108 ppm, with R2 values exceeding 0.99. The LOD was 0.9 ppm and the LOQ was 2.6 ppm for frozen tuna, which gave the lowest background level of contaminant. Cross-reactivity of the assay was tested against 14 other biogenic amines and was found to be minimal for all (<0.5%), except for agmatine (4.1%) and putrescine (0.9%). There was no observable interference from any tested biogenic amines. Product consistency was verified by validating lot-to-lot variations and variations within the same lot. Overall recoveries for all tested matrixes were within the acceptable range (80–120%). A 1-year claimed shelf life of the kit at 4°C was verified by accelerated stability study data collected on days 1, 15, and 32 at 25°C and by real-time stability testing at 1-month, 6-month, and 1-year at 4°C. No difference in histamine detection was observed in ruggedness testing, in which minor changes were introduced to the assay protocol. Good agreement was observed between AOAC Official MethodSM977.13 and the MaxSignal® Histamine Enzymatic Assay method. Independent laboratory testing demonstrated that the MaxSignal method works with the same precision in the hands of minimally trained technicians as with the expert method developers. This study validates the performance of Bioo Scientific’s rapid enzymatic method.

Determination of histamine in canned tuna fish available in Tehran market by ELISA method

2020 ◽  
Author(s):  
Naficeh Sadeghi ◽  
Masoomeh Behzad ◽  
Behrooz Jannat ◽  
Mohammad Reza Oveisi ◽  
Mannan Hajimahmoodi ◽  
...  
Keyword(s):  
Biogenic Amines ◽  
Enzyme Linked Immunosorbent Assay ◽  
Elisa Method ◽  
Average Amount ◽  
Histamine Concentration ◽  
Tuna Fish ◽  
Canned Tuna ◽  
Canned Fish ◽  
Standard Limit

Histamine is one of the well-known biogenic amines and responsible for causing allergic reactions. The presence of biogenic amines in the foodstuff is harmful, if it enters in a large amount to blood. In sea-food products, due to lack of proper storage at appropriate temperatures (freezing), histamine may be formed and will remain in the product, since it is already dry and heat resistance. Hazard of histamine consumption and average amount of canned fish consumed worldwide makes histamine measurement in canned fish very important. In this study 56 samples from 22 different brands were assessed and Enzyme-Linked Immunosorbent Assay (ELISA) was used by spectrophotometry for histamine detection. Our study showed that histamine levels in canned fish available in Tehran market, though it is high (5.75±5.98 mg/100 g tuna), but is not in a hazardous state (p<0.01). Our research showed that lowest and highest histamine concentration were 2.14 ±0.17 and 21.69±0.11 mg/100 g of fish respectively. It also indicates that medium does not affect the histamine content. There were no significant differences in the samples of fish and tuna fish for histamine. The amount of histamine in the tuna was below the standard limit (<50 mg histamine/100 g). Further studies should be carried out to investigate the presence of histamine in various fish and other sea-food.

Validation Study of a HistaSure™ ELISAFast Track for the Determination of Histamine in Fish Samples

2014 ◽  
Vol 97 (6) ◽  
pp. 1601-1614 ◽  
Author(s):  
Georg Manz ◽  
Esther Booltink
Keyword(s):  
Fish Meal ◽  
Cross Reactivity ◽  
Fluorometric Method ◽  
Canned Tuna ◽  
Acceptable Range ◽  
Accelerated Stability ◽  
Fish Samples ◽  
Fresh Frozen ◽  
Aoac Official

Abstract LDN Labor Diagnostika Nord GmbH & Co. KG has developed an ELISA for the rapid semiquantitative or quantitative determination of histamine in different kinds of fish samples. Fresh/frozen tuna, canned tuna, fresh/frozen mahi mahi, canned sardines, and fish meal were used to validate the method under the requirements of the AOAC Research Institute Performance Tested MethodsSM Program. The results all fell within the defined acceptance criteria. Linearity was given throughout the 0–300 ppm measuring range. Cross reactivity to similarly structured food spoilage indicators (tyramine and cadaverine) was minimal, less than 1%. Overall recoveries for all tested matrixes were within the determined acceptable range (80–120%), and the repeatability of precision was less than 10% overall and less than 5% at the defect action level of 50 ppm set by the U.S. Food and Drug Administration. The LOQ for the ELISA was determined to be 1.27 ppm. No lot-to-lot differences were observed. A 2-year claimed shelf life, at 2–8°C, was confirmed through accelerated stability testing. After the introduction of minor procedural variations to the test, no differences in histamine levels were observed. Independent lab testing revealed that the ELISA works as well in the hands of minimally trained technicians as it does with expert developers. A strong correlation (r = 0.97) between the LDN ELISA and the AOAC 977.13 fluorometric method was observed. This study revealed that the LDN ELISA is equivalent to the AOAC Official Method977.13 for the precise and accurate measurement of histamine in fresh/frozen tuna, canned tuna, fresh/frozen mahi mahi, canned sardines, and fish meal.

Human Prothrombin Activation: Determination of Plasma and Serum Levels of Prothrombin Fragment 3 by Radioimmunoassay

1979 ◽  
Author(s):  
Daniel Walz ◽  
Thomas Brown
Keyword(s):  
Blood Clotting ◽  
Factor Xa ◽  
Heart Association ◽  
Serum Levels ◽  
Cross Reactivity ◽  
Assay Procedure ◽  
A Chain ◽  
Prothrombin Activation ◽  
Theoretical Amount

Human prothrombin activation is unique in that, in addition to the release of fragment 1.2 (FI.2) from the NH-terminus of prothrombin by factor Xa during the generation of thrombin, an additional 13 residue polypeptide, fragment 3 (F3), is autocatalytically removed from the amino-terminus of the thrombin A chain. We have developed a rapid radioimmunoassay for human F3 which incorporates short incubation times and the use of a preprecipitated second antibody; the assay can be performed in three hours. Specificity studies in buffer systems show prothrombin and prethrombin 1 cross-reacting at a level of 0.001; purified thrombin does not cross-react. In the presence of 5% BSA, prothrombin displays considerably less cross-reactivity. No immunoreactive material to F3 antibodies could be detected in 400 μL of plasma. Serum, obtained from whole blood clotting, contained measurable quantities of F3 (40-100 ng/mL). This amount in serum represents only 5-10% of the theoretical amount available should all of the fragment be hydrolytically cleaved during the conversion of prothrombin to thrombin. This assay procedure is currently being utilized to monitor the activation of purified human prothrombin in the absence and presence of selected plasma inhibitors. (Supported in part by NIH 05384-17 and the Michigan Heart Association).

Development of Validated Stability Indicating HPTLC Method for Assay of Ozagrel and its Pharmaceutical Formulations

2018 ◽  
pp. 36-48 ◽  
Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production ◽  
Hptlc Method

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

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.

Determination of biogenic amines in tomato by ion-pair chromatography coupled to an amine-selective potentiometric detector

2021 ◽  
pp. 138134
Author(s):  
Renato L. Gil ◽  
Célia G. Amorim ◽  
Maria C.B.S.M. Montenegro ◽  
Alberto N. Araújo
Keyword(s):  
Biogenic Amines ◽  
Ion Pair ◽  
Ion Pair Chromatography
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