scholarly journals Dissipation Kinetics and the Pre-Harvest Residue Limits of Acetamiprid and Chlorantraniliprole in Kimchi Cabbage Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2616
Author(s):  
Jonghwa Lee ◽  
Byung Joon Kim ◽  
Eunhye Kim ◽  
Jeong-Han Kim
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Dissipation Kinetics ◽  
Relative Standard ◽  
Harvest Residue

The dissipation behaviors of acetamiprid and chlorantraniliprole in kimchi cabbages were studied under open-field conditions. A simple and rapid analytical method was developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The multiple reaction monitoring (MRM) conditions of two pesticides were optimized to quantify and identify the pesticide residues. Sample preparation was performed by the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. Average recovery rates at the different spiked levels (0.05 and 0.25 mg/kg) were in the range of 103.6–113.9% (acetamiprid) and 80.8–91.2% (chlorantraniliprole), and the relative standard deviations were ≤4.3% for all. The dissipation kinetics were assessed using first-order equations after spraying acetamiprid and chlorantraniliprole individually on kimchi cabbages. The biological half-lives in field 1 and 2 were 5.2 and 6.3 days (acetamiprid) and 10.0 and 15.2 days (chlorantraniliprole), respectively. Based on the dissipation equations, the pre-harvest residue limits (PHRLs) corresponding to each day before harvest were suggested as the guidelines to meet the MRL on harvest day. It was also predicted that the terminal residues observed after multiple sprayings (three and seven days) would be below the MRL when harvested, in compliance with the established pre-harvest intervals.

scholarly journals Pharmacokinetics of isocorynoxeine in rat plasma after intraperitoneal administration by UPLC–MS/MS

2020 ◽  
Vol 32 (4) ◽  
pp. 260-263
Author(s):  
Haichao Zhan ◽  
Zhen Wei ◽  
Ke Ren ◽  
Shuhua Tong ◽  
Xianqin Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Intraperitoneal Administration ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Isocorynoxeine is one of the main alkaloids in Chinese medicinal herbs, and has pharmacological activities such as antihypertensive, sedative, anticonvulsant, and neuronal protection. It is an effective component of Uncaria for the treatment of hypertension. In this study, we used a fast and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect isocorynoxeine in rat plasma and investigated its pharmacokinetics in rats. Six rats were given isocorynoxeine (15 mg/kg) by intraperitoneal (i.p.) administration. Blood (100 μL) was withdrawn from the caudal vein at 5 and 30 min and 1, 2, 4, 6, 8, 12, and 24 h after administration. Chromatographic separation was achieved using a UPLC BEH C18 column using a mobile phase of acetonitrile–0.1% formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in the multiple reaction monitoring (MRM) mode with positive ionization was applied. Intra-day and inter-day precisions (relative standard deviation, %RSD) of isocorynoxeine in rat plasma were lower than 12%. The method was successfully applied in the pharmacokinetics of isocorynoxeine in rats after intraperitoneal administration. The t1/2 of isocorynoxeine is 4.9 ± 2.1 h, which indicates quick elimination.

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 Pharmacokinetics and bioavailability of hapepunine in mice by ultra-performance liquid chromatography–tandem mass spectrometry

2020 ◽  
Vol 32 (1) ◽  
pp. 44-48
Author(s):  
Lianguo Chen ◽  
Qingwei Zhang ◽  
Yijing Lin ◽  
Xiaojie Lu ◽  
Zuoquan Zhong ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Ultra Performance Liquid Chromatography ◽  
Absolute Bioavailability ◽  
Tandem Mass ◽  
Mouse Blood ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine the hapepunine in mouse blood, and the pharmacokinetics of hapepunine after intravenous (1.0 mg/kg) and intragastric (2.5, 5, and 10 mg/kg) administrations was studied. Delavinone was used as an internal standard. The UPLC ethylene bridged hybrid (BEH) C18 column was used for chromatographic separation. The mobile phase consisted of acetonitrile and 0.1% formic acid with a gradient elution flow rate of 0.4 mL/min. Multiple reaction monitoring (MRM) mode was used for quantitative analysis of hapepunine in electrospray ionization (ESI) positive interface. Proteins from mouse blood were removed by acetonitrile precipitation. The verification method was established in accordance with the US Food and Drug Administration (FDA) bioanalytical method validation guidelines. In the concentration range of 1–1000 ng/mL, the hapepunine in the mouse blood was linear (r2 > 0.995), and the lower limit of quantification was 1.0 ng/mL. In the mouse blood, the intra-day precision coefficient of variation (CV) was less than 12%, the inter-day precision CV was less than 14%. The accuracy ranged from 91.7% to 109.3%. The average recovery was higher than 76.7%, and the matrix effect was between 86.0% and 106.4%. The UPLC–MS/MS method was sensitive, rapid, and selective and was successfully applied to the pharmacokinetic study of hapepunine in mice. The absolute bioavailability of hapepunine was 22.0%.

scholarly journals Detection and Identification of Zeranol in Chicken or Rabbit Liver by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

2002 ◽  
Vol 85 (4) ◽  
pp. 841-847 ◽  
Author(s):  
Xiaoming Fang ◽  
Jiahua Chen ◽  
Dehua Guo ◽  
Guoquan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Rabbit Liver ◽  
Negative Ion ◽  
Tandem Mass ◽  
Detection And Identification ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A sensitive, specific, and reliable liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detection and identification of zeranol in chicken or rabbit liver. A homogenized liver sample was hydrolyzed with β-glucuronidase/arylsulfatase, and the hydrolysate was extracted with ethyl ether. The supernatant was evaporated to dryness, and the residue was dissolved in chloroform and re-extracted with sodium hydroxide. After acidification, the extract was cleaned up on a C18 solid-phase extraction cartridge and analyzed by electrospray LC-MS/MS in the negative ion mode. The multiple reaction monitoring transition from both m/z 321 to 277 and m/z 321 to 303 was monitored for confirmation, and the product ion of 277 was used for quantitation. Separation was performed on a Waters XTettra™ C18 column (50 × 2.1 mm, 3.5 μm) combined with a safeguard column (Symmetry C18, 20 × 3.9 mm, 5 μm), using a gradient elution with acetonitrile and 20mM ammonium acetate. Calibration curves were prepared and good linearity was achieved over the concentration ranges tested. For all liver samples fortified at 3 different levels of 1, 5, and 50 μg/kg, the overall recoveries and relative standard deviations were in the range of 61–90 and 8–13%, respectively. The limit of quantitation based on the assay validation was 1 μg/kg. The method had been used on a routine basis for detection and identification of zeranol in liver samples.

scholarly journals Distribution of Polyphenolic and Isoprenoid Compounds and Biological Activity Differences between in the Fruit Skin + Pulp, Seeds, and Leaves of New Biotypes of Elaeagnusmultiflora Thunb

Antioxidants ◽  
2021 ◽  
Vol 10 (6) ◽  
pp. 849
Author(s):  
Sabina Lachowicz-Wiśniewska ◽  
Ireneusz Kapusta ◽  
Carla M. Stinco ◽  
Antonio J. Meléndez-Martínez ◽  
Anna Bieniek ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Photodiode Array Detection ◽  
Fruit Skin ◽  
Liquid Chromatography Tandem Mass

The purpose of this study was to determine the distribution of polyphenolic and isoprenoid compounds and organic acids in the fruit skin + pulp, seeds, and leaves of six new biotypes of Elaeagnus multiflora Thunb., as well as their in vitro biological potency. The polyphenols and isoprenoids were determined with UPLC-PDA-MS/MS (ultra-performance liquid chromatography coupled to photodiode array detection and electrospray ionization tandem mass spectrometry) and RRLC-MS/MS (rapid resolution liquid chromatography/tandem mass spectrometry) methods, the organic acid with HPLC-RID (high-performance liquid chromatography coupled to a Refractive Index Detector), and the antioxidant capacity using ABTS and FRAP assays. Enzymatic activity was established as the ability to inhibit α-amylase, α-glucosidase, and pancreatic lipase. Owing to such an effective technique, 88 compounds were recorded, with 17 polyphenolic compounds and 3 isoprenoids identified for the first time in the seeds and leaves of cherry silverberry. In total, 55 compounds were identified in the leaves, 36 in the seeds, and 31 in the fruit skin + pulp. The predominant polyphenol was polymeric procyanidin (66–95% of total polyphenolics), whereas the predominant isoprenoids were chlorophyll b and (all-E)-lycopene. The results of our work noted that there are significant differences in the profiles of several secondary metabolites between the analyzed parts of the plant, and depending on the need, the compounds can be used to develop different innovative food or cosmetic products.

A Sensitive Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry Method Based on Derivatization with 1-Nitro-2-Naphthaldehyde for Determination of Alkylhydrazines in Surface water

2021 ◽  
Author(s):  
Jin-Ah Oh ◽  
Ho-Sang Shin ◽  
Hyun-Hee Lim
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Surface Water ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Abstract Background Alkylhydrazines are widely used in the industrial fields. An analysis of alkylhydrazines in surface water is need because these chemicals are likely to be discharged into wastewater and enter aquatic environments. Objective An ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed to determine the levels of five alkylhydrazines (N,N-dimethylhydrazine, ethylhydrazine, 1-isopropylhydrazine, phenylhydrazine and 1-methyl-1-phenylhydrazine) in surface water. Methods This method is based on the derivatization of alkylhydrazines with 1-nitro-2-naphthaldehyde (NNA) in water. A derivatization reagent dosage of 0.5 mg of NNA, a pH of 2, and a reaction time of 30 min at 40 °C were determined to be the optimal conditions for UHPLC–MS/MS detection. The derivatives were injected into the LC system without additional extraction or purification steps. Results The proposed method was used under optimized conditions to detect alkylhydrazines in surface water, with the limit of quantification found to be 0.01–0.03 μg/L. The accuracy ranged from 91.0 to 106.0%, and the precision, expressed as the relative standard deviation, was less than 10%. Of the five alkylhydrazines, only N,N-dimethyl hydrazine was detected in the real samples at a concentration range of 0.010 to 0.041 μg/L. Conclusion The developed method can be used to confirm the presence of alkylhydrazine residues in surface water and represents an important tool for evaluating the fate of alkylhydrazines in surface water. Highlights This method to determine alkylhydrazine in surface water was developed simply and rapidly after derivatization reaction without an extraction or clean-up step in UHPLC-MS/MS.

scholarly journals A Validated Method for the Simultaneous Determination of Methamphetamine and 3,4-Methylenedioxy-N-methamphetamine in Blood-Based Liquid Chromatography-Tandem Mass Spectrometry

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Dinh-Vu Le ◽  
Trong-Tuan Nguyen ◽  
Van-Trong Nguyen
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been validated for the simultaneous determination of methamphetamine (MA) and 3,4-methylenedioxy-N-methamphetamine (MDMA) in the blood sample. Under the optimal experimental conditions, the concentration of MA can be determined in the range from 1 µg/L to 5000 µg/L with the method detection limit (MDL) of 0.31 µg/L. The range from 0.5 to 500 µg/L is observed for the determination of MDMA with the MDL down to 0.25 µg/L. The practical applicability of the method is performed with the recovery ranging from 85.3% to 94% for MA and from 86.9% to 95.5% for MDMA. At the different concentrations of drugs, the relative standard deviations (RSD) for both MA and MDMA are lower than 5.7%. The method was applied to analyse 1995 blood samples that had been collected from the Forensic Medicine Centre of Ho Chi Minh City. The results showed 1.75% positive with MA and 0.25% positive with MDMA. These two drugs take 10% of the total drugs positive samples. By using deuterium-labelled methamphetamine-d5 and 3,4-methylenedioxy-N-methamphetamine-d5 as the internal standards in the determination and the use of MS/MS in multiple reaction monitoring mode signal readout, the method exhibits robustness specificity and can be applied in simultaneous determination of MA and MDMA in blood with high selectivity and sensitivity.

scholarly journals Simultaneous determination of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi using ultra-performance liquid chromatography/tandem mass spectrometry

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Fajun Tian ◽  
Chengkui Qiao ◽  
Caixia Wang ◽  
Jing Luo ◽  
Linlin Guo ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Edible Fungi ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

AbstractA fast, sensitive, and reliable analytical method was developed and validated for simultaneous identification and quantification of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi by ultra-performance liquid chromatography/tandem mass spectrometry (UHPLC–MS/MS). First, sample extraction was done with acetonitrile containing 1% formic acid followed by phase separation with the addition of MgSO4:NaOAc. Then, the supernatant was purified by primary secondary amine (PSA), octadecylsilane (C18), and graphitized carbon black (GCB). The linearities of the calibrations for all analytes were excellent (R2 ≥ 0.9953). Acceptable recoveries (74.5–106.4%) for all analytes were obtained with good intra- and inter- relative standard deviations of less than 14.5%. The limit of quantification (LOQs) for all analytes was 10 μg kg−1. For accurate quantification, matrix-matched calibration curve was applied to normalize the matrix effect. The results indicated that the method was suitable for detecting the three acaricides and their relevant metabolites in edible fungi.

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