Determination of Neonicotinoid Insecticides and their Metabolites, and Strobilurin Fungicides in Atmospheric Particles using Liquid Chromatography-Positive Electrospray Ionization-Tandem Mass Spectrometry

2021 ◽  
Vol 6 (1) ◽  
Author(s):  
Behdarvandan A ◽  
◽  
Raina Fulton R ◽  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Atmospheric Particles ◽  
Tandem Mass ◽  
Particle Phase ◽  
Neonicotinoid Insecticides ◽  
Strobilurin Fungicides ◽  
Relative Standard

A liquid chromatography-tandem mass spectrometry method has been developed for the simultaneous determination of metabolites of neonicotinoid insecticides with neonicotinoid insecticides and strobilurin fungicides in the particle phase fraction of atmospheric samples. Pressurized solvent extraction was used to extract the target analytes from particles collected on glass fiber filters, followed by a C18 SPE cleanup step. Recoveries of 85.9 to 108.3% and relative standard deviation <13% were obtained for all analytes. The method detection limit for metabolites of neonicotinoid insecticides were 0.5-3 ng/ mL (air concentrations of 0.44-2.66 pg/m³). Matrix effects were compensated for using standard addition calibration for quantitation. This paper provides the first detection of desmethyl-thiamethoxam which coincided with higher concentrations of thiamethoxam in atmospheric particles. Other neonicotinoid insecticides and strobilurin fungicides detected in the particle phase in the atmosphere included acetamiprid, clothianidin, imidacloprid, azoxystrobin, kresoxim-methyl, pyraclostrobin, and trifloxystrobin. This research highlights the potential of not only neonicotinoid insecticides and strobilurin fungicides moving in the atmosphere in the particle phase, but also a metabolite of thiamethoxam (desmethyl-thiamethoxam) in a region with orchards and vineyards where foliar applications with air blast sprayers dominate.

scholarly journals Liquid Chromatography–Tandem Mass Spectrometry for the Simultaneous Determination of Doxorubicin and its Metabolites Doxorubicinol, Doxorubicinone, Doxorubicinolone, and 7-Deoxydoxorubicinone in Mouse Plasma

Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1254 ◽  
Author(s):  
Won-Gu Choi ◽  
Dong Kyun Kim ◽  
Yongho Shin ◽  
Ria Park ◽  
Yong-Yeon Cho ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Tandem Mass ◽  
Mouse Plasma ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Doxorubicin, an anthracycline antitumor antibiotic, acts as a cancer treatment by interfering with the function of DNA. Herein, liquid chromatography-tandem mass spectrometry was for the first time developed and validated for the simultaneous determination of doxorubicin and its major metabolites doxorubicinol, doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The liquid–liquid extraction of a 10 μL mouse plasma sample with chloroform:methanol (4:1, v/v) and use of the selected reaction monitoring mode led to less matrix effect and better sensitivity. The lower limits of quantification levels were 0.5 ng/mL for doxorubicin, 0.1 ng/mL for doxorubicinol, and 0.01 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone. The standard curves were linear over the range of 0.5–200 ng/mL for doxorubicin; 0.1–200 ng/mL for doxorubicinol; and 0.01–50 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The intra and inter-day relative standard deviation and relative errors for doxorubicin and its four metabolites at four quality control concentrations were 0.9–13.6% and –13.0% to 14.9%, respectively. This method was successfully applied to the pharmacokinetic study of doxorubicin and its metabolites after intravenous administration of doxorubicin at a dose of 1.3 mg/kg to female BALB/c nude mice.

Simultaneous Determination of Isopyrazam and Azoxystrobin in Cucumbers by Liquid Chromatography–Tandem Mass Spectrometry

2017 ◽  
Vol 80 (12) ◽  
pp. 2112-2118 ◽  
Author(s):  
Dan Hu ◽  
Xu Xu ◽  
Tian Cai ◽  
Wei-Ying Wang ◽  
Chun-Jie Wu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effects ◽  
Fast Method ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

ABSTRACTA rapid and sensitive analytical method based on high-performance liquid chromatography–tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg−1 (n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg−1, respectively, which are far below the maximum residue level (0.5 mg kg−1) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

Determination of Diflubenzuron Residues in Vegetables by UPLC-MS/MS

2014 ◽  
Vol 852 ◽  
pp. 266-269
Author(s):  
Xiao Fang Wang ◽  
Chun Liang Yang ◽  
Mao Fang Huang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

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.

scholarly journals Simultaneous determination of seven glucocorticoids in cosmetics by liquid chromatography tandem mass spectrometry

2020 ◽  
Vol 3 (2) ◽  
pp. 115-124
Author(s):  
Dong Bui Quang ◽  
Phuong Vu Thi ◽  
Van Anh Tran Thi ◽  
Son Tran Cao ◽  
◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Fluocinolone Acetonide ◽  
Tandem Mass ◽  
Chromatography Method ◽  
Relative Standard

A rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) was developed and validated for the simultaneous determination of 7 glucocorticoids (GC) including hydrocortisone acetate (HCA), cortisone acetate (COA), prednisone (PDS), prednisolone (PDL), methyl prednisolone (MPL), dexamethasone (DEX) and fluocinolone acetonide (FLA), which may be illegally blended in transdermal cosmetics. Sample preparation step consists of the extraction with ethyl acetate followed by centrifugation and filtration. The extract was dried, diluted and cleaned using C18 SPE column. The compounds were separated by reversed-phase chromatography with mobile phase containing 0.1% formic acid in water and acetonitrile in gradient condition. The method was validated at the validation level from 0.12 to 6.0 &micro;g/g. The LODs for PDS, PDL and FLA were 0.3 &micro;g/g and for the others were 0.03 &micro;g/g, and LOQs were 0.6 and 0.12 &micro;g/g, respectively. The reproducibility was satisfied with the relative standard deviation below 23% and the recoveries were in the range of 74.3-106.7% meeting AOAC requirements. The studied glucocorticoids were detected in about 20% of tested samples collected in Hanoi with the level contents in the range from 0.18 to 16.2 &micro;g/g.

scholarly journals Simultaneous Determination of 17 Sulfonamides and the Potentiators Ormetoprim and Trimethoprim in Salmon Muscle by Liquid Chromatography with Tandem Mass Spectrometry Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 343-348 ◽  
Author(s):  
Ross A Potter ◽  
B Garth Burns ◽  
Jeffrey M van de Riet ◽  
David H North ◽  
Rozina Darvesh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Fish Tissue ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Relative Standard

Abstract A simple, robust method using liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of 17 sulfonamides sulfanilamide (SNL), sulfacetamide (SAA), sulfaguanidine (SGD), sulfapyridine (SPY), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethoxazole (SOZ), sulfamoxole (SXL), sulfisoxazole (SXZ), sulfamethizole (SML), sulfamethazine (SMZ), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfachloropyridazine (SCP), sulfaquinoxaline (SQX), and sulfadimethoxine (SDM) and 2 potentiators ormetoprim (OMP) and trimethoprim (TMP) in fish tissue has been developed. The analytes were extracted from homogenized fish tissue with wateracetonitrile (50 + 50). The extract was clarified by centrifugation and a portion defatted with hexane. The analytes were partitioned into chloroform and evaporated to dryness. The redissolved residue was applied to a C18 reversed-phase column with a wateracetonitrile (0.1% acetic acid) gradient. All of the compounds were completely separated and detected in &lt;10 min at 30°C using LC/MS/MS. Standard curves were linear over the range of 0.02 to 5 ng injected. The limit of detection varied from 0.1 ng/g for SMZ and OMP to 0.9 ng/g for SXL and SOZ. Recoveries varied from 100% for SDM, SOZ, and SQX and 85% for SMR, OMP, and TMP to approximately 30% for SAA. Relative standard deviations for repeat analysis varied from 4% for SMZ and SCP to 23% for SAA.

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