scholarly journals Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4975
Author(s):  
Xuan Zhang ◽  
Yunhua Hui ◽  
Changling Fang ◽  
Yuan Wang ◽  
Feng Han ◽  
...  

A sensitive and reliable method was developed to determine methylene blue (MB) and its metabolite residues, including azure A (AZA), azure B (AZB), and azure C (AZC) in aquatic products by HPLC–MS/MS. The samples were extracted by acetonitrile and cleaned up by alumina-neutral (ALN) cartridges. The analytes were separated on a Sunfire C18 column (150 mm × 2.1 mm, 5 µm). The method was validated according to the European criteria of Commission Decision 2002/657/CE. Good linearity between 1–500 µg/L was obtained with correlation coefficients (R2) greater than 0.99. The limit of quantification (LOQ) was 1.0 µg/kg. The average recoveries at three levels of each compound (1, 5, and 10 µg/kg) were demonstrated to be in the range of 71.8–97.5%, with relative standard deviations (RSDs) from 1.05% to 8.63%. This method was suitable for the detection of methylene blue and its metabolite residues in aquatic products.

2014 ◽  
Vol 852 ◽  
pp. 266-269
Author(s):  
Xiao Fang Wang ◽  
Chun Liang Yang ◽  
Mao Fang Huang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  

The conditions for detecting residues of diflubenzuron in vegetables by ultra high performance liquid chromatography tandem mass spectrometry were studied. The target was extracted with acetonitrile for 2 min with a homogenizer. The extaction was purifide by a conditioned Florisil SPE cartridge, and then was detected by ultra high-performance liquid chromatography with tandem mass spectrometry. The average recovery was in the range from 87.8 %- 99.2 % at spike levels of 0.1, 1.0 and 10 mg/kg in vegetables, and relative standard deviations was in the range of 4.2 %-8.9 %. The proposed method is fast, simple, sensitive and accurate.


2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.


2019 ◽  
Vol 82 (7) ◽  
pp. 1160-1165 ◽  
Author(s):  
TAO GUO ◽  
XIAOLI WANG ◽  
HAIFENG WANG ◽  
YUFEN HU ◽  
SHIYONG ZHANG ◽  
...  

ABSTRACTAn effective method for determination of multiple residues of phenoxy acid herbicides in cereals was developed. A QuEChERS (quick, easy, cheap, effective, rugged, and safe) technique coupled with high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) was optimized for the analysis of phenoxy acid herbicides in rice, corn, and wheat. The limits of detection in the experiment were 0.0500 μg/kg for 4-(2,4-dichlorophenoxy)acetic acid, (4-chloro-2-methylphenoxy)acetic acid, (2,4,5-trichlorophenoxy)acetic acid, and 2-(2,4-dichlorophenoxy)propionic acid and 0.300 μg/kg for 4-(2,4-dichlorophenoxy)butyric acid and 3,6-dichloro-2-methoxybenzoic acid. The relative standard deviation of intraday and interday precision for the six phenoxy acid herbicides was less than 6.61%, and accuracy was 96.3 to 107%. Extraction recovery for phenoxy acid herbicides was 73.8 to 115%, with relative standard deviations of less than 12.1% at three spiking levels (1.00, 4.00, and 20.0 μg/kg). These results indicate that QuEChERS sample preparation with HPLC-MS/MS analysis is a rapid, reliable, highly sensitive, and specific tool for the determination of phenoxy acid herbicide residues in cereals.HIGHLIGHTS


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