A Method for Determination of Penicillin G Residue in Waste Penicillium chrysogenum Using High Performance Liquid Chromatography

2015 ◽  
Vol 768 ◽  
pp. 15-24
Author(s):  
Pu Wang ◽  
Hui Ling Liu ◽  
Bing Wang ◽  
Xiu Wen Cheng ◽  
Qing Hua Chen ◽  
...  

In this study, a rapid and selective method has been developed to determine PENG residues in waste penicillium chrysogenum by using SPE cleanup strategy followed by HPLC. Furthermore, some parameters which influenced the extraction efficiency including extraction mode, solvent and time, while washing solution and eluting solution for SPE were systematically investigated. It should be noted that the extraction process was carried out in a single step by mixing the extraction solvent acetonitrile: formic acid in aqueous solution and chrysogenum samples under ultrasound. The SPE procedure was conducted using Oasis HLB as the clean up cartridge, n-hexane as washing solution, and mixture of acetonitrile and methanol as eluting solution. Under the optimized conditions, the linear of PENG are in the range of 0.1-2000 μg/mL, with the correlation was R2>0.99. In addition, the recoveries of PENG in these samples at three fortification levels of 800-1800mg/kg were 74.98% to 113.47% are obtained, respectively. Moreover, a limits of detection (0.006 mg/kg) and quantification (0.02 mg/kg) could be achieved.

Author(s):  
Klaudia Kokoszka ◽  
Agnieszka Kobus ◽  
Sylwia Bajkacz

The residues of antimicrobials used in human and veterinary medicine are popular pollutants of anthropogenic origin. The main sources of introducing antimicrobials into the environment are sewage treatment plants and the agricultural industry. Antimicrobials in animal manure contaminate the surrounding soil as well as groundwater, and can be absorbed by plants. The presence of antimicrobials in food of plant origin may pose a threat to human health due to their high biological activity. As part of the research, a procedure was developed for the extraction and determination of ciprofloxacin, enrofloxacin, cefuroxime, nalidixic acid and metronidazole in environmental samples (soil and parsley root). An optimized solid-liquid extraction (SLE) method was used to separate antimicrobials from the solid samples and a mixture of citrate buffer (pH = 4): methanol (1:1; v/v) was used as the extraction solvent. Solid phase extraction (SPE) with OASIS® HLB cartridges was used to purify and pre-concentrate the sample. The recovery of the developed method was in the range of 55–108%. Analytes were determined by high-performance liquid chromatography coupled with an ultraviolet (UV) detector and a tandem mass spectrometer (HPLC-UV-MS/MS). The procedure was validated and applied to the determination of selected antimicrobials in soil and parsley root samples. Five types of soil and five types of parsley roots of different origins were analyzed. The presence of nalidixic acid in the parsley root samples was found in the concentration range of 0.14–0.72 ng g−1. It has been shown that antimicrobials are absorbed by the plant and can accumulate antimicrobials in its edible parts.


2003 ◽  
Vol 66 (8) ◽  
pp. 1439-1443 ◽  
Author(s):  
JEONG-HUN KANG ◽  
FUSAO KONDO

This study was conducted to develop a selective and sensitive method for the determination of bisphenol A (BPA) levels in milk and dairy products. A method based on solvent extraction with acetonitrile and solid-phase extraction (SPE) was developed for the analysis of BPA in milk, yogurt, cream, butter, pudding, condensed milk, and flavored milk, and a method using two SPE cartridges (OASIS HLB and Florisil cartridge) for skim milk was also developed. The developed methods showed good recovery levels (77 to 102%) together with low detection limits (1 μg/liter for milk, yogurt, pudding, condensed milk, flavored milk, and skim milk and 3 μg/liter for cream and butter). These methods are simple, sensitive, and suitable for the analysis of BPA in milk and dairy products. When 40 milk and dairy products were analyzed by the proposed methods, BPA was not identified in noncanned products, but its levels ranged from 21 to 43 μg/kg in canned products, levels that were 60- to 140-fold lower than the migration limits in the European Union and Japan.


Toxins ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 583 ◽  
Author(s):  
Zhihong Xuan ◽  
Jin Ye ◽  
Bing Zhang ◽  
Li Li ◽  
Yu Wu ◽  
...  

Sample clean-up remains the most time-consuming and error-prone step in the whole analytical procedure for aflatoxins (AFTs) analysis. Herein, an automated and high-throughput sample clean-up platform was developed with a disposable, cost-effective immunoaffinity magnetic bead-based kit. Under optimized conditions, the automated method takes less than 30 min to simultaneously purify 20 samples without requiring any centrifugation or filtering steps. When coupled to ultra-high performance liquid chromatography with fluorescence detection, this new analysis method displays excellent accuracy and precision as well as outstanding efficiency. Furthermore, an interlaboratory study was performed in six laboratories to validate the novel protocol. Mean recovery, repeatability, reproducibility, and Horwitz ratio values were within 91.9%–107.4%, 2.5%–7.4%, 2.7%–10.6%, and 0.26%–0.90, respectively. Results demonstrate that the developed sample clean-up platform is a reliable alternative to most widely adopted clean-up procedures for AFTs in cereals and oils.


2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Min Zhao ◽  
Xianhui Li ◽  
Di Zhang ◽  
Longshan Zhao

Objective. To establish a method for extraction and determination of antioxidant 264 (2,6-di-tert-butyl-4-methylphenol) in the brominated butyl rubber stopper for injection and migration study in recombinant potent antitumor and antivirus protein injection (Novaferon). Methods. Dichloromethane-ethanol was adopted as the extraction solvent during the process of reflux extraction of antioxidant 264 in the brominated butyl rubber stopper. High-performance liquid chromatography (HPLC) was used for the determination of the migration of antioxidant 264 to Novaferon. The mobile phase consisted of acetonitrile-water (80 : 20, v/v). The flow rate was 1.5 mL/min. The detection wavelength was 280 nm. Results. The linearity range was from 4.003 to 200.150 μg/mL (r2 = 0.99996), and the average recovery of antioxidant 264 was 97.8%. The applicability of the methodology was good, which can be used for the determination of antioxidant 264. The results indicated that antioxidant 264 was not detected in Novaferon after the accelerated test and three months of long-term test. Conclusion. The established validated method in this study can be used for the determination of antioxidant 264 in the rubber stopper, and the brominated butyl rubber stopper has good compatibility with Novaferon.


2013 ◽  
Vol 718-720 ◽  
pp. 219-222
Author(s):  
Jia Qi Ju ◽  
Zhong Hang Wu ◽  
Zhen Liu Chen ◽  
Zhi Jiang He ◽  
Long He ◽  
...  

This research developed and optimized the methods for simultaneous determination of tetracycline (TCs), macrolide (MLs) and sulfonamide (SAs) antibiotics in soils using accelerated solvent extraction (ASE)- solid-phase extraction (SPE)-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methanol-citric acid (pH=4.7) was used as extraction solvent, diatomite (washed by EDTA) was used as dispersing agent. Firstly, soil was extracted by ASE with the parameter conditions: pressure 1500 psi, temperature 70°C, static 10 min, 1 circle, then pre-concentration by SPE and followed by HPLC-MS/MS analysis. Recovery was 86.3%~97.4% for SAs, 67.3%~87.4% for TCs and 68.4%~78.3% for MLs. RSD < 9 % and r > 0.99. Limits of detection (LOD) was 0.5~0.9 ug/kg for SAs, 0.2~1.1 ug/kg for TCs and 0.2~0.3 ug/kg for MLs. This method determined 9 kinds of antibiotics within 15 min, the determination accuracy can meet the requirements of actual analysis.


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