Development of One-Step Non-Solvent Extraction and Sensitive UHPLC-MS/MS Method for Assessment of N-(n-Butyl) Thiophosphoric Triamide (NBPT) and N-(n-Butyl) Phosphoric Triamide (NBPTo) in Milk

N-(n-butyl) thiophosphoric triamide (NBPT) is a urease inhibitor utilised in urea-based fertilizers. In Ireland, fertilizer treated with NBPT is applied to pasture to mitigate both ammonia and nitrous oxide emissions, but concerns arise as to the potential for residues in milk products. A quick ultrafiltration extraction and ultra-high performance liquid chromatography coupled with mass spectrometry triple quadrupole (UHPLC-MS/MS) quantitation method was developed and validated in this study. The method was applied in the analysis of samples collected from a field study investigating potential transfer of NBPT residues into milk. NBPT and NBPTo residues, were extracted from fortified milk samples and analysed on a UHPLC-MS/MS with recoveries ranging from 74 to 114%. Validation of the UHPLC-MS/MS method at low (0.0020 mg kg−1) and high (0.0250 mg kg−1) concentration levels in line with SANTE/12682/2019 showed overall trueness in the range of 99 to 104% and precision between 1 and 10%, RSD for both compounds. The limit of quantitation (LOQ) was 0.0020 mg kg−1 and other tested parameters (linearity, sensitivity, specificity, matrix effect, robustness, etc.) satisfied acceptance criteria. Stability assessment using spiked samples revealed the compounds were stable in raw and pasteurised milk for 4 weeks at –80 °C storage temperature. Maintaining samples at pH 8.5–9.0 further improved stability. Analysis of 516 milk samples from the field study found that NBPT and NBPTo concentrations were below the LOQ of 0.0020 mg kg−1, thus suggesting very low risk of residues occurring in the milk. The method developed is quick, robust, and sensitive. The method is deemed fit-for-purpose for the simultaneous determination of NBPT and NBPTo in milk.

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Optimization and Validation of a Multiclass Screening and Confirmation Method for Drug Residues in Milk Using High-Performance Liquid Chromatography/Tandem Mass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/94.2.383 ◽

2011 ◽

Vol 94 (2) ◽

pp. 383-393 ◽

Cited By ~ 15

Author(s):

Susan B Clark ◽

Joseph M Storey ◽

Sherri B Turnipseed

Keyword(s):

High Performance ◽

Screening Method ◽

Veterinary Drug ◽

Drug Residues ◽

Milk Samples ◽

Safe Level ◽

Fortified Milk ◽

Liquid Chromatography Tandem Mass ◽

New Compounds ◽

Positive Controls

Abstract The further optimization and validation of a multiresidue veterinary drug screening method for milk is described. The drug residues of regulatory interest in milk include -lactams, sulfonamides, tetracyclines, fluoroquinolones, and macrolides. A previously published procedure has been modified to incorporate new compounds and to collect both screening and confirmatory ion transitions in one acquisition method. Milk samples were extracted with an equal volume of acetonitrile. The samples were then subjected to cleanup with a bonded SPE cartridge and a MW cutoff filter. The SPE protocol was modified to effectively recover a metabolite of flunixin. Established tolerance levels are set for most of these drugs in milk; thus, the screening procedure was semiquantitative, using positive controls for comparison. The positive controls, consisting of extracts from milk fortified with the drugs at their tolerance or safe level, were used to set statistically valid minimum response criteria for unknown samples. This updated method was validated with fortified milk, as well as with milk samples from animals administered veterinary drugs.

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PREPARATION AND STABILITY EVALUATION OF LL-37 CREAM

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2021v13i6.39639 ◽

2021 ◽

pp. 139-143

Author(s):

ELIZA MIRANDA ◽

KUSMARINAH BRAMONO ◽

LUDDWI ACHMAD RIZKY ◽

HAYUN

Keyword(s):

Chromatographic Analysis ◽

Mobile Phase ◽

High Performance ◽

Room Temperature ◽

Limit Of Detection ◽

Stability Evaluation ◽

C Storage ◽

Limit Of Quantitation ◽

Photodiode Array ◽

Physical Changes

Objective: The present study aimed to prepare LL-37 in a cream formulation (O/W emulsion) and evaluate its stability by determining the physical changes in the cream and concentration of LL-37 using validated high-performance liquid chromatography. Methods: The method was conducted at room temperature using a C18 column (5 µm × 250 mm × 4.6 mm) as a stationary phase, a mixture of 0.1% trifluoroacetic acid (TFA)/water (A) and 0.1% TFA/acetonitrile (B) (85:15) as the mobile phase, a flow rate of 1.0 mL/min, and photodiode array set at 228 nm as the detector. The method was validated in compliance with the Association of Official Analytical Chemists and International Conference on Harmonization guidelines. It demonstrated excellent linearity, accuracy, precision, specificity, the limit of detection, and limit of quantitation. Results: The chromatographic analysis indicated minimal degradation of LL-37 during the 12-week, with a predicted expiry time of 99 and 75 mo stored at 4 °C and 28 °C, respectively. Conclusion: LL-37 cream establishes good physical characteristics and stabilizes the active ingredient, especially at 4 °C and 28 °C storage. Therefore, the emulsion delivery system of LL-37 cream is harmless and stable as a novel alternative vehicle of LL-37.

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Properties of New Strawberry Lines Compared with Well-Known Cultivars in Winter Planting System Conditions

Notulae Botanicae Horti Agrobotanici Cluj-Napoca ◽

10.15835/nbha45110477 ◽

2017 ◽

Vol 45 (1) ◽

pp. 9-16 ◽

Cited By ~ 4

Author(s):

Leo SABATINO ◽

Claudio DE PASQUALE ◽

Farid ABOUD ◽

Federico MARTINELLI ◽

Matteo BUSCONI ◽

...

Keyword(s):

High Performance ◽

Storage Temperature ◽

Field Performance ◽

Fruit Production ◽

Temperature Treatment ◽

Primary Objective ◽

Fruit Storage ◽

Quality Properties ◽

C Storage ◽

Physical And Chemical Quality

In Southern Italy and Sicily, strawberry cultivation is dominated by international cultivars such as ‘Candonga Sabrosa’, ‘Florida Fortuna’, ‘Sabrina’ and ‘Sant Andreas’. The primary objective of our study was to compare the field performance of two experimental lines and four established cultivars in a Sicilian representative strawberry production area. The second objective was to compare the fruits physic-chemical nutraceutical characteristics of these genotypes in response to different postharvest fruit storage temperatures. A supporting genetic analysis, via SSR markers, was also performed in order to establish genotype correlations. Our study confirmed the high result of ‘Florida Fortuna’ in terms of earliness and productivity and the high performance of ‘Candonga Sabrosa’ in terms of total soluble content and fruit firmness. The new lines ‘PA1’ and ‘PA2’ showed satisfying results. However, the new line ‘PA2’, might deserve particular attention by growers involved in strawberry early fruit production in Mediterranean areas both for its yield performance and fruit quality characteristics. This study also showed that a 4 °C fruit storage temperature treatment for 36 hours positively affects the physical and chemical quality properties of strawberry fruits, whereas overall quality declines at 20 °C storage. According to the genetic characterization, ‘PA2’ was closely related to ‘Candonga Sabrosa’ and ‘Florida Fortuna’.

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Navel Orange Pitting Stimulated by Waxing and High Storage Temperature

HortScience ◽

10.21273/hortsci.33.3.520b ◽

1998 ◽

Vol 33 (3) ◽

pp. 520b-520

Author(s):

Huating Dou ◽

Peter D. Petracek ◽

Craig Davis

Keyword(s):

High Temperature ◽

Storage Temperature ◽

Chilling Injury ◽

Citrus Fruit ◽

Navel Orange ◽

Oil Glands ◽

C Storage ◽

High Storage Temperature ◽

Florida Citrus ◽

Citrus Varieties

Navel oranges are reportedly susceptible to postharvest peel disorders, including chilling injury and aging/stem end rind breakdown. These and other physiological disorders are sometimes given the common term “navel rind breakdown.” California citrus industry reports on recent incidences of navel rind breakdown suggested that some instances of this disorder were similar to “postharvest pitting,” a disorder that we have observed in a number of Florida citrus varieties. Thus, we decided to define the morphology and etiology of pitting of `Washington' navel orange (Citrus sinensis L.) peel. The disorder was characterized by the collapse of clusters of oil glands and was stimulated by wax application and high temperature (≥13 °C) storage. Internal ethanol levels of waxed fruit stored at high temperature (13 or 21 °C) were significantly higher among fruit that developed pitting than those that did not. The pitting observed in these studies is comparable to previously observed navel orange disorders that have occurred without known cause. Navel orange pitting is morphologically and etiologically distinct from chilling injury and aging/stem end rind breakdown, but is similar to postharvest pitting of Florida citrus fruit.

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Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

Current Pharmaceutical Analysis ◽

10.2174/1573412914666171228163122 ◽

2019 ◽

Vol 15 (3) ◽

pp. 273-279

Author(s):

Shweta G. Rangari ◽

Nishikant A. Raut ◽

Pradip W. Dhore

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Degradation Products ◽

Analysis Data ◽

Peak Height ◽

Good Resolution ◽

Stability Indicating ◽

Limit Of Quantitation ◽

Wide Range ◽

Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

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Phycocyanin content and nutritional profile of Arthrospira platensis from Mexico: efficient extraction process and stability evaluation of phycocyanin

BMC Chemistry ◽

10.1186/s13065-021-00746-1 ◽

2021 ◽

Vol 15 (1) ◽

Author(s):

Sanghamitra Khandual ◽

Edgar Omar Lopez Sanchez ◽

Hugo Espinosa Andrews ◽

Jose Daniel Padilla de la Rosa

Keyword(s):

Storage Temperature ◽

Extraction Process ◽

Arthrospira Platensis ◽

Extraction Methods ◽

Precipitation Method ◽

Partial Purification ◽

Natural Food ◽

Solvent Ratio ◽

C Storage ◽

Dry Biomass

AbstractPhycocyanin is a blue natural food colorant with multiple health benefits. Here we propose an efficient phycocyanin extraction method from Arthrospira platensis from Mexico. Three extraction methods were applied to optimize the extraction process, using water and buffer as solvents, with three pH values at two agitation times. The highest phycocyanin, 54.65 mg/g, was extracted from dry biomass with water as a solvent using an ultrasonication bar. The optimum condition of extraction was determined to be 1:50 biomass/solvent ratio for dry biomass, with the freeze/thaw method for 20 min repeated twice, and then agitated at 120 rpm for 24 h. The phycocyanin content was 48.88 mg/g biomass, with a purity of 0.47. For scalable phycocyanin productivity, the sonication method is recommended as there is no statistical difference. The phycocyanin stability was best at − 20 °C storage temperature at pH 7 for 35 days. Partial purification with ammonium sulfate was found to be suitable as a fractional precipitation method, first at 0–20% and then 20–65%, to get purity nearly 1. Total protein was found to be 55.52%, and total amino acids after phycocyanin extraction was 33%. The maximum phycocyanin yield using water as a solvent was the most interesting result regardless of the method used for extraction.

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High-Performance Lead-Acid Batteries Enabled by Pb and PbO2 Nanostructured Electrodes: Effect of Operating Temperature

Applied Sciences ◽

10.3390/app11146357 ◽

2021 ◽

Vol 11 (14) ◽

pp. 6357

Author(s):

Roberto Luigi Oliveri ◽

Maria Grazia Insinga ◽

Simone Pisana ◽

Bernardo Patella ◽

Giuseppe Aiello ◽

...

Keyword(s):

High Performance ◽

Active Material ◽

Active Surface ◽

Effect Of Temperature ◽

Active Surface Area ◽

Polycarbonate Membrane ◽

Nanostructured Electrodes ◽

Lead Acid Batteries ◽

Improved Stability ◽

Lead Acid

Lead-acid batteries are now widely used for energy storage, as result of an established and reliable technology. In the last decade, several studies have been carried out to improve the performance of this type of batteries, with the main objective to replace the conventional plates with innovative electrodes with improved stability, increased capacity and a larger active surface. Such studies ultimately aim to improve the kinetics of electrochemical conversion reactions at the electrode-solution interface and to guarantee a good electrical continuity during the repeated charge/discharge cycles. To achieve these objectives, our contribution focuses on the employment of nanostructured electrodes. In particular, we have obtained nanostructured electrodes in Pb and PbO2 through electrosynthesis in a template consisting of a nanoporous polycarbonate membrane. These electrodes are characterized by a wider active surface area, which allows for a better use of the active material, and for a consequent increased specific energy compared to traditional batteries. In this research, the performance of lead-acid batteries with nanostructured electrodes was studied at 10 C at temperatures of 25, −20 and 40 °C in order to evaluate the efficiency and the effect of temperature on electrode morphology. The batteries were assembled using both nanostructured electrodes and an AGM-type separator used in commercial batteries.

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A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2019v11i5.33281 ◽

2019 ◽

pp. 60-65

Author(s):

MADHURIMA BASAK ◽

Santhosh Reddy Gouru ◽

Animesh Bera ◽

Krishna veni Nagappan

Keyword(s):

Quantitative Analysis ◽

High Performance ◽

Dosage Form ◽

Limit Of Detection ◽

Hplc Method ◽

Reverse Phase ◽

Pharmaceutical Dosage Form ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

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Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

SLAS TECHNOLOGY Translating Life Sciences Innovation ◽

10.1177/2472630320982308 ◽

2021 ◽

pp. 247263032098230

Author(s):

Dilshad Ahmad ◽

Faisal A. Al Meshaiti ◽

Yazeed K. Al Anazi ◽

Osama Al Owassil ◽

Alaa Eldeen B. Yassin

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Reversed Phase ◽

Hplc Method ◽

Hybrid Nanoparticles ◽

Array Detector ◽

Relative Standard ◽

Validation Parameters ◽

Limit Of Quantitation ◽

Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

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Growth and enterotoxin production of Bacillus cereus in cow, goat, and sheep milk

Acta Veterinaria Brno ◽

10.2754/avb201483s10s3 ◽

2014 ◽

Vol 83 (10) ◽

pp. S3-S8 ◽

Cited By ~ 5

Author(s):

Lenka Necidová ◽

Šárka Bursová ◽

Alena Skočková ◽

Bohdana Janštová ◽

Pavla Prachařová ◽

...

Keyword(s):

Bacillus Cereus ◽

Storage Temperature ◽

Goat Milk ◽

Storage Conditions ◽

Cow Milk ◽

Enzyme Linked Immunosorbent Assay ◽

Plate Method ◽

Milk Samples ◽

Sheep Milk ◽

Enterotoxin Production

The aim of this study was to compare Bacillus cereus growth rates and diarrhoeal enterotoxin production in raw and pasteurized goat, sheep, and cow milk in terms of storage conditions. Milk samples were inoculated with B. cereus (CCM 2010), which produces diarrhoeal enterotoxins. Enterotoxin production was tested by ELISA (Enzyme-Linked Immunosorbent Assay), and the count of B. cereus was determined by the plate method. With raw cow milk, B. cereus growth and enterotoxin production can be completely suppressed; in raw goat and sheep milk, enterotoxin was produced at 22 °C. In pasteurized cow, goat, and sheep milk, the B. cereus count increased under all storage conditions, with more rapid growth being observed at 15 °C (sheep milk) and 22 °C (cow and goat milk). Enterotoxin presence was detected at 15 °C and 22 °C, and with pasteurized cow milk also at 8 °C. Our model experiments have determined that B. cereus multiplication and subsequent enterotoxin production depend on storage temperature and milk type.

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