scholarly journals Effective and rugged analysis of glyphosate, glufosinate, and metabolites in Tenebrio molitor larva (mealworms) using liquid chromatography tandem mass spectrometry

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Leesun Kim ◽  
Sujn Baek ◽  
Kyungae Son ◽  
Hee-Dong Lee ◽  
Dal-Soon Choi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tenebrio Molitor ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Food And Feed

AbstractTenebrio molitor larva (mealworms) has recently attracted attention as a protein source for food and feed. The larva is generally fed with wheat bran, which can be possibly contaminated with glyphosate. To establish food safe standards, a rugged and effective analytical method for glyphosate, aminomethylphosphonic acid, glufosinate, and their metabolites including 3-methylphosphinico-propionic acid, and N-acetyl glufosinate, in mealworms was optimized using liquid chromatography tandem mass spectrometry. An anionic polar pesticide column was used due to its high suitability for glyphosate. Acidified water and acetonitrile were used to extract the target compounds without contribution from various fatty and pigment interferences derived from brownish insects. Seven different clean-up procedures ((1) 50 mg C18 (2) 20 mg C18/Z-sep (3) PRiME hydrophilic-lipophilic balance (HLB) cartridge (4) 75 mg Z-sep, (5) 75 mg Z-sep+, (6) EMR-lipid cartridge, and (7) 50 mg ENVI-Carb) were compared. Due to its simplicity and cost-effectiveness, PRiME HLB was selected for clean-up. The recoveries of the target compounds were ranged from 86 to 96% with < 20% relative standard deviations. Therefore, this simple and effective method can be applied for the two pesticides and their metabolites in other edible insects or high-fat matrices.

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 Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3210 ◽  
Author(s):  
Michele Protti ◽  
Camilla Marasca ◽  
Marco Cirrincione ◽  
Angelo E. Sberna ◽  
Roberto Mandrioli ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Anabolic Androgenic Steroids ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Androgenic Steroids

Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine.

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 Ochratoxin A in Wine by Immunoaffinity Cleanup and Liquid Chromatography Tandem Mass Spectrometry

2008 ◽  
Vol 71 (5) ◽  
pp. 1038-1042 ◽  
Author(s):  
SHIGEKUNI NOBA ◽  
MASAYUKI OMOTE ◽  
YASUSHI KITAGAWA ◽  
NAOKI MOCHIZUKI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ochratoxin A ◽  
Tandem Mass ◽  
Immunoaffinity Column ◽  
White Wines ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A simple and accurate method has been developed for determining ochratoxin A (OTA), using an immunoaffinity column for cleanup and liquid chromatography–tandem mass spectrometry for identification and quantification. Wine samples were diluted with a solution containing polyethylene glycol 8000 and sodium hydrogen carbonate, filtered through a glass microfiber filter, and cleaned up on an immunoaffinity column. OTA was then eluted with methanol–acetic acid (98:2) and analyzed by liquid chromatography–tandem mass spectrometry. The average recoveries of OTA from red and white wines were 95 and 96.7% (spiked OTA level was 0.05 ng/ml) and repeatabilities (relative standard deviation) were 3.8 and 2.4%, respectively. The detection limit was 0.0003 ng/ml based on the signal-to-noise ratio in wine of 3:1. Analysis of 74 samples of domestic and imported wines showed OTA levels ranging from &lt;0.0003 to 0.82 ng/ml, with an incidence of contamination of 92.1% for red wines, and &lt;0.0003 to 0.51 ng/ml, with an incidence of contamination of 77.8% for white wines. These detection rates were higher than those rates of past reports of OTA contamination in wine, due to the high sensitivity of this method. However, all samples analyzed in this study complied with European Union regulations. It is concluded that this method is a useful tool for the quality assurance of wine.

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 sixteen illegal dyes in foodstuffs by liquid chromatography tandem mass spectrometry

2020 ◽  
Vol 3 (1) ◽  
pp. 1-10
Author(s):  
Phuong Vu Lan ◽  
Ha Binh Nguyen Thi ◽  
Huyen Doan Thu ◽  
Kim Van Le Thi ◽  
Son Tran Cao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Sudan I ◽  
Liquid Chromatography Tandem Mass ◽  
Auramine O ◽  
Chili Powder

A liquid chromatography tandem mass spectrometry method using positiveelectrospray ionization source (ESI+), multiple reaction monitoring (MRM) mode has been developed and validated to simultaneously determine 16 illegaldyes in different food groups. The method was based on the extraction of analytes from samples using QuEChERS technique. After being cleaned up d-SPE tube with mixture of MgSO4, PSA and C18 sorbent, the extract was analyzed by LC-MS/MS. Each illegaldyewas characterized by a precursor ion and two product ions. The method allows the screening of the simultaneous presence of 16 illegal substances at the lowest concentration of 5&micro;g/kg forrhodamin B, crystal violet, chrysoidine G, auramine O, sudan black B, pararosanilin and of 50&micro;g/kg for remaining substances. The specificity of the methodmet 657/2002/EC requirements. The methodwas linear in the range from 1-1000&micro;g/L and themethod detection limit was from 5-50 &micro;g/kg, the recovery ranged from 73-104% and the relative standard deviations were lower than 16.4%. The method has been applied to analyze 30 samples of dried beef, dry chicken, chutney, chili powder and food coloring samples. Rhodamine B, sudan I and auramine O were detected in two chili powder and 04 food coloring samples.

scholarly journals Simultaneous Quantification of Chloramphenicol, Thiamphenicol, Florfenicol, and Florfenicol Amine in Animal and Aquaculture Products Using Liquid Chromatography-Tandem Mass Spectrometry

2022 ◽  
Vol 8 ◽  
Author(s):  
Hae-Ni Jung ◽  
Da-Hee Park ◽  
Yeon-Jae Choi ◽  
Se-Hyeong Kang ◽  
Hee-Jung Cho ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Linear Matrix ◽  
Tandem Mass ◽  
Simultaneous Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Aquaculture Products

The accumulation of antimicrobial residues in edible animal products and aquaculture products could pose health concerns to unsuspecting consumers. Hence, this study aimed to develop a validated method for simultaneous quantification of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in beef, pork, chicken, shrimp, eel, and flatfish using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Primary-secondary amine (PSA) and MgSO4 were used for sample purification. The analytes were separated on a reversed-phase analytical column. The coefficients of determination for the linear matrix-matched calibration curves were ≥0.9941. Recovery rates ranged between 64.26 and 116.51% for the four analytes with relative standard deviations (RSDs) ≤ 18.05%. The calculated limits of detection (LODs) and limits of quantification (LOQs) were 0.005–3.1 and 0.02–10.4 μg/kg, respectively. The developed method was successfully applied for monitoring samples obtained from local markets in Seoul, Republic of Korea. The target residues were not detected in any tested matrix. The designed method was versatile, sensitive, and proved suitable for quantifying residues in animal-derived products.

scholarly journals Disperse Solid-Phase Extraction Cleanup for the Determination of 1-Deoxynojirimycin in Mulberry Leaves with Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Lei Zhang ◽  
Yiran Zhou ◽  
Jing Meng ◽  
Jia Li
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Good Precision ◽  
Mulberry Leaves ◽  
Water Solvent ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A new determination method of 1-deoxynojirimycin (1-DNJ) in mulberry leaves based on ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed. Dried and crushed mulberry leaves’ sample was extracted by MeCN-water solvent, purified by graphitized carbon black (GCB) and primary secondary amine (PSA) to remove organic acids and pigments, and then analyzed after attenuation and filtration. The calibration curve showed linearity in the concentration range of 10–500 ng/mL, with the correlation coefficient of 0.998. Recoveries of spiked 1-DNJ at three fortification levels ranged from 94.6% to 96.4%, with relative standard derivation below 1.2%. Additionally, the matrix effect was assessed as negligible. Compared with methods by gas chromatography (GC) and liquid chromatography (LC) via real sample detection, the proposed method acquired better stability and detection efficiency. These results proved that this method has advantages of simple operation, complete purification, small pretreatment loss, good precision and accuracy, and high determination specificity, which is suitable for massive monitoring and precise quantitation of 1-DNJ in mulberry leaves.

scholarly journals Liquid Chromatography/Tandem Mass Spectrometry Analysis of Chloramphenicol in Cooked Crab Meat

2005 ◽  
Vol 88 (4) ◽  
pp. 1155-1159 ◽  
Author(s):  
Heidi S Rupp ◽  
James S Stuart ◽  
Jeffrey A Hurlbut
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Mass Spectrometry Analysis ◽  
Tandem Mass ◽  
Spectrometry Analysis ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Crab Meat

Abstract A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method is described for the extraction, cleanup, determination, and confirmation of chloramphenicol (CAP) in cooked crab meat. The method involves pulverization of cooked crab meat with dry ice; extraction of the CAP into ethyl acetate (EtOAc); evaporation (by N2) of the EtOAc; addition of methanol, aqueous NaCl, and heptane; extraction of the lipids into the heptane, followed by extraction of the aqueous phase with EtOAc; evaporation (by N2) of the EtOAc; dissolution into methanol–water; filtration; and separation/detection/confirmation using LC/MS/MS. Crab meat was fortified at 0.25, 0.50, and 1.0 ng/g (ppb) chloramphenicol. Average absolute recoveries were 67, 84, and 86%, respectively, with relative standard deviation values all less than 1%. Four daughter ions (m/z 152, 176, 194, and 257) were monitored off the m/z 321 precursor ion. Determination was based on a standard curve using the peak areas of the m/z 152 daughter ion (the base peak) for standard solutions equivalent to 0.10, 0.20, 0.50, and 1.0 ppb in tissue (made with control crab extract). A set of 6 matrix controls (unfortified crab meat) was also analyzed, in which no chloramphenicol was detected. For identification purposes, the ion ratios (of each daughter ion versus the base daughter ion) of the fortified crab versus those of the chloramphenicol standards agreed within 10% (relative) at fortified chloramphenicol concentrations of 0.25–1.0 ppb.

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