Dissipation rate of acetamiprid in sweet cherries

Degradation of acetamiprid in sweet cherry samples was evaluated at several intervals from the product application until the end of the pre-harvest interval. An orchard of sweet cherries located at Stepanovicevo village near Novi Sad was used in this study. Acetamiprid was applied according to the manufacturer?s recommendation for protecting sweet cherries from their most important pests. Sweet cherry fruit samples were collected at eight intervals: immediately after acetamiprid application and 2, 4, 6, 8, 10, 12 and 14 days after application. The extraction of acetamiprid from sweet cherry samples was performed using a QuEChERS-based method. Determination was carried out using an HPLC-UV diode array detection system (Agilent 1100, United States) with an Agilent Zorbax Eclipse C18 column (50 mm C 4.6 mm internal diameter, 1.8 ?m particle size). The method was subjected to a thorough validation procedure. The recovery data were obtained by spiking blank sweet cherry samples at three concentration levels (0.1-0.3 mg/ kg), yielding 85.4% average recovery. Precision values expressed as relative standard deviation (RSD) were below 1.61% for the intraday precision. Acetamiprid showed linear calibrations from 0.05 to 2.5 ?g/ml with correlation coefficient (R2) of 0.995%. The limit of detection and limit of quantification were found to be 5 ?g/kg and 14 ?g/kg, respectively. The validated method was applied in the analysis of acetamiprid in sweet cherry samples. During the study period, the concentration of acetamiprid decreased from 0.529 mg/kg to 0.111 mg/kg. The content of acetamiprid in sweet cherry samples at the end of the pre-harvest interval was below the maximum permissible level specified by the Serbian and EU MRLs.

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Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

Open Chemistry ◽

10.1515/chem-2020-0102 ◽

2020 ◽

Vol 18 (1) ◽

pp. 962-973

Author(s):

Saira Arif ◽

Sadia Ata

Keyword(s):

Mobile Phase ◽

Limit Of Detection ◽

Fluocinolone Acetonide ◽

Internal Diameter ◽

Forced Degradation ◽

Specific Method ◽

Regression Equations ◽

Limit Of Quantification ◽

Simultaneous Quantification ◽

Relative Standard

AbstractA rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

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Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

Current Pharmaceutical Analysis ◽

10.2174/1573412916666200210150914 ◽

2020 ◽

Vol 16 ◽

Author(s):

Nadereh Rahbar ◽

Fatemeh Ahmadi ◽

Zahra Ramezani ◽

Masoumeh Nourani

Keyword(s):

Human Serum ◽

High Performance ◽

Limit Of Detection ◽

Solid Phase ◽

Nano Particles ◽

Limit Of Quantification ◽

Analytical Methodology ◽

Fiber Fabrication ◽

Relative Standard ◽

Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

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A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

Future Journal of Pharmaceutical Sciences ◽

10.1186/s43094-020-00175-2 ◽

2021 ◽

Vol 7 (1) ◽

Author(s):

Indhu Priya Mabbu ◽

G. Sumathi ◽

N. Devanna

Keyword(s):

Method Development ◽

Limit Of Detection ◽

Vinyl Sulfone ◽

Limit Of Quantification ◽

Relative Standard ◽

Pressure Chemical Ionization ◽

Pressure Chemical ◽

Development And Validation ◽

Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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A highly sensitive octopus-like azobenzene fluorescent probe for determination of abamectin B1 in apples

Scientific Reports ◽

10.1038/s41598-021-84221-w ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Zhenlong Guo ◽

YiFei Su ◽

Kexin Li ◽

MengYi Tang ◽

Qiang Li ◽

...

Keyword(s):

Fluorescent Probe ◽

Limit Of Detection ◽

Quantitative Detection ◽

Fluorescence Signal ◽

Ionization Mass ◽

Limit Of Quantification ◽

Visible Absorption ◽

Esi Ms ◽

Relative Standard ◽

Ft Ir

AbstractThe development of detecting residual level of abamectin B1 in apples is of great importance to public health. Herein, we synthesized a octopus-like azobenzene fluorescent probe 1,3,5-tris (5′-[(E)-(p-phenoxyazo) diazenyl)] benzene-1,3-dicarboxylic acid) benzene (TPB) for preliminary detection of abamectin B1 in apples. The TPB molecule has been characterized by ultraviolet–visible absorption spectrometry, 1H-nuclear magnetic resonance, fourier-transform infrared (FT-IR), electrospray ionization mass spectroscopy (ESI-MS) and fluorescent spectra. A proper determination condition was optimized, with limit of detection and limit of quantification of 1.3 µg L−1 and 4.4 μg L−1, respectively. The mechanism of this probe to identify abamectin B1 was illustrated in terms of undergoing aromatic nucleophilic substitution, by comparing fluorescence changes, FT-IR and ESI-MS. Furthermore, a facile quantitative detection of the residual abamectin B1 in apples was achieved. Good reproducibility was present based on relative standard deviation of 2.2%. Six carboxyl recognition sites, three azo groups and unique fluorescence signal towards abamectin B1 of this fluorescent probe demonstrated reasonable sensitivity, specificity and selectivity. The results indicate that the octopus-like azobenzene fluorescent probe can be expected to be reliable for evaluating abamectin B1 in agricultural foods.

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Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽

10.3390/molecules26071837 ◽

2021 ◽

Vol 26 (7) ◽

pp. 1837

Author(s):

Harischandra Naik Rathod ◽

Bheemanna Mallappa ◽

Pallavi Malenahalli Sidramappa ◽

Chandra Sekhara Reddy Vennapusa ◽

Pavankumar Kamin ◽

...

Keyword(s):

Limit Of Detection ◽

Solid Phase ◽

Graphitized Carbon Black ◽

Limit Of Quantification ◽

Gas And Liquid Chromatography ◽

Relative Standard ◽

The Matrix ◽

Liquid Chromatography Tandem Mass ◽

Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

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Gold-nanourchin complexed silicon dioxide-probe on gap-fingered interdigitated electrode surface for Parkinson’s Disease determination by current–volt measurement

Nanomaterials and Nanotechnology ◽

10.1177/1847980420987352 ◽

2021 ◽

Vol 11 ◽

pp. 184798042098735

Author(s):

Xiaohong Li ◽

Wei Shi ◽

Wenyan Zhang ◽

Weiyao Chen ◽

Dan Cao ◽

...

Keyword(s):

Parkinson’S Disease ◽

Parkinson's Disease ◽

Silicon Dioxide ◽

Limit Of Detection ◽

Detection System ◽

Interdigitated Electrode ◽

Limit Of Quantification ◽

Neurofilament Light Chain ◽

Neurofilament Light ◽

Detection Range

Parkinson’s disease (PD) is a nervous disorder, affects physical movement, and leads to difficulty in balancing, walking, and coordination. A novel sensor is mandatory to determine PD and monitor the progress of the treatment. Neurofilament light chain (NfL) has been recognized as a good biomarker for PD and also helps to distinguish between PD and atypical PD syndromes. Immunosensor was generated by current–volt measurement on gap-fingered interdigitated electrode with silicon dioxide surface to determine NfL level. To enhance the detection, anti-NfL antibody was complexed with gold-nanourchin and immobilized on the sensing electrode. The current–volt response was gradually increased at the linear detection range from 100 fM to 1 nM. Limit of detection and sensitivity were 100 fM with the signal-to-noise ratio at n = 3 on a linear curve ( y = 0.081 x + 1.593; R 2 = 0.9983). Limit of quantification falls at 1 pM and high performance of the sensor was demonstrated by discriminating against other neurogenerative disease markers, in addition, it was reproducible even in serum-spiked samples. This method of detection system aids to measure the level of NfL and leads to determine the condition with PD.

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Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa100 ◽

2020 ◽

Author(s):

Murat Soyseven ◽

Rüstem Keçili ◽

Hassan Y Aboul-Enein ◽

Göksel Arli

Keyword(s):

Analytical Method ◽

High Performance ◽

Orthophosphoric Acid ◽

Limit Of Detection ◽

Detection System ◽

Active Pharmaceutical Ingredient ◽

Limit Of Quantification ◽

Column Temperature ◽

Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

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SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2017v9i2.16828 ◽

2017 ◽

Vol 9 (2) ◽

pp. 34

Author(s):

N. Balaji ◽

Sayeeda Sultana

Keyword(s):

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

High Performance Liquid Chromatographic ◽

Hplc Method ◽

Internal Diameter ◽

Related Substances ◽

Relative Standard ◽

Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

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Determination of uric acid in human serum by an enzymatic method using N-methyl-N-(4-aminophenyl)-3-methoxyaniline reagent

Journal of the Serbian Chemical Society ◽

10.2298/jsc0309691j ◽

2003 ◽

Vol 68 (8-9) ◽

pp. 691-698 ◽

Cited By ~ 7

Author(s):

Milena Jelikic-Stankov ◽

Predrag Djurdjevic ◽

Dejan Stankov

Keyword(s):

Uric Acid ◽

Human Serum ◽

Limit Of Detection ◽

Ascorbate Oxidase ◽

Acid Oxidation ◽

Uric Acid Concentration ◽

Enzymatic Method ◽

Limit Of Quantification ◽

Relative Standard

In this work a new enzymatic method for the determination of uric acid in human serum has been developed. The method is based on the oxidative coupling reaction between the N-methyl-N-(4-aminophenyl)-3-methoxyaniline (NCP) reagent and the hydrogen ? donor reagent N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-methylaniline (TOOS), in the system involving three enzymes: uricase, peroxidase and ascorbate oxidase. Using this method uric acid could be determined in concentrations up to 1.428 mmol/L, with a relative standard deviation of up to 1.8 %. The effect of the medium pH and the NCP concentration on the linearity of the chromogen absorbance versus the uric acid concentration curve was investigated. The influence of the uricase activity on the maximum rate of uric acid oxidation was also examined. The use of the NCP reagent demonstrated a more precise and more sensitive determination of the uric acid compared to the determination with 4-aminoantipyrine (4-AA) as the coupling regent. The sensitivity of the method determined from the calibration curve was 0.71 absorbance units per mmol/L of uric acid; the limit of detection was LOD = 0.0035 mmol/L and the limit of quantification was LOQ = 0.015 mmol/L of uric acid.

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Application of RP-HPLC for the Estimation of Allopurinol and Its Related Substances in Bulk and Tablet Dosage Form

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i20b31354 ◽

2021 ◽

pp. 11-20

Author(s):

Ch. Jaswanth Kumar ◽

Prachet Pinnamaneni ◽

Siva Prasad Morla ◽

K. N. Rajini Kanth ◽

Rama Rao Nadendla

Keyword(s):

Drug Testing ◽

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Limit Of Quantification ◽

Related Substance ◽

Related Substances ◽

Rp Hplc ◽

Relative Standard ◽

Tablet Dosage

Aims: The main aim of the present study was to develop and validate a simple and cost- effective method for the estimation of allopurinol and its related substances by using RP-HPLC. Study Design: Estimation of Allopurinol and its related substance in bulk and tablet dosage forms by RP-HPLC. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute of Pharmaceutical Sciences, Chalapathi Nagar, Lam, Guntur-522034 between October 2020 to January 2021. Methodology: Method development was carried out by using Schimadzu, Prominence-i series LC 3D-Plus autosampler embedded with lab solutions software, equipped with PDA detector using YMC column (150 mm X 4.6 mm, 3 μm) and 0.1M Ammonium acetate buffer as a mobile phase in the ratio of 100% at a flow rate of 1.0 ml/min at a wavelength of 255nm. The developed method was validated according to ICH guidelines. Results: The linearity was observed in the range of 20-100 µg/ml with a regression (R2) value of 0.999. Developed method was specific with no interactions and accurate with 100.11% for allopurinol and 99.54% for its related substance. The limit of detection for allopurinol was 2 µg/ml and for related substance was 0.0.1 µg/ml. The limit of quantification for allopurinol was 6 µg/ml and for related substance was 0.03 µg/ml respectively. The percentage relative standard deviation was found to be NMT 2 which indicates that the proposed method was precise and robust. Conclusion: The developed method was simple, precise and accurate and can be successfully employed for the estimation of allopurinol in bulk and tablet dosage form.

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