Single-Laboratory Validation of a Multi-residue Method for Simultaneous Analysis of Multi-class Pesticides in Turmeric by Liquid Chromatography Tandem Mass Spectrometry

2020 ◽  
Author(s):  
Bappa Ghosh ◽  
Arijita Bhattacharyya ◽  
Sandip Hingmire ◽  
Pushpa Aher ◽  
Pradnya Zende ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Residue Analysis ◽  
High Throughput Analysis ◽  
Method Performance ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Powder Samples ◽  
First Time

Abstract Background For years, turmeric has been used in several cuisines worldwide because of its proven health benefits. However, as its cultivation often involves applications of polar and semi-polar pesticides, their residues might cause health hazards to consumers. The dearth of a validated LC-MS/MS method for the residue analysis of these pesticides in turmeric has warranted the present study. Objective The aim was to develop and validate a multi-residue method for simultaneous determination of multi-class pesticides in turmeric (both rhizome and powder) by LC-MS/MS. Method Both the rhizome and powder samples (1 kg) were soaked in water for 30 min, followed by homogenization. Each homogenate (2 g) was mixed with 10 mL water, and extracted with acetonitrile (10 mL) in the presence of acetic acid and NaCl. The extract was cleaned by using dispersive solid phase extraction (dSPE) with graphitized carbon (5 mg/mL) sorbent. The cleaned extract was measured by LC-MS/MS with a runtime of 20 min. The method was validated on 211 multi-class pesticides. Results The method performance was satisfactory at 10 ng/g and higher levels, in compliance with the SANTE/12682/2019 guidelines. The dSPE cleanup was effective in minimizing the matrix effects. The use of matrix-matched calibrations specific for turmeric powder and rhizome corrected all recoveries within the satisfactory range of 70–120%. The precision -RSDs were <20% for all test pesticides. The Horwitz ratio and measurement uncertainty results were satisfactory as well. Conclusions As the method was convenient, selective, accurate, and repeatable, it is recommended for regulatory and commercial testing purposes. Highlights For the first time, this study reports a validated LC-MS/MS method for the multi-residue analysis of pesticides in turmeric. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision. The method performance satisfied the requirements of the SANTE/12682/2019 guidelines, and the method sensitivity complied with the EU-MRL requirements.

Multi-residue Analysis of Pesticides in Turmeric (Powder and Rhizome) Using Gas Chromatography Tandem Mass Spectrometry

2020 ◽  
Vol 103 (6) ◽  
pp. 1498-1511 ◽  
Author(s):  
Bappa Ghosh ◽  
Narayan Kamble ◽  
Arijita Bhattacharyya ◽  
Chandrasekar Kandaswamy ◽  
Kaushik Banerjee
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Residue Analysis ◽  
Graphitized Carbon Black ◽  
High Throughput Analysis ◽  
Accuracy And Precision ◽  
Quality Control Criteria ◽  
Primary Secondary Amine ◽  
Fit For Purpose ◽  
Control Criteria

Abstract Background and objectives Turmeric is widely used as an ingredient of food and medicinal products. There exists no validated method for multi-residue analysis of pesticides in turmeric. Objective This study was undertaken to develop a simple and robust method for the quantitative determination of multi-class pesticides in turmeric powder and rhizome by GC-MS/MS. Method Initially, the samples were soaked in water for 30 min and homogenized to a fine paste. A portion of this paste (2 g) was extracted with acetonitrile (2 mL) and partitioned with hexane (2 mL) after adding 5 mL of 20% NaCl. The cleanup step involved dispersive solid phase extraction with graphitized carbon black (GCB, 5 mg/mL). Its performance was evaluated against primary secondary amine (PSA) and C18 sorbents. The cleaned extract was evaporated to dryness and reconstituted in ethyl acetate before GC-MS/MS analysis. The method was validated for a mixture of 208 multi-class pesticides at 10 ng/g and higher levels (i.e., 20 and 50 ng/g). Results The findings, which demonstrated a satisfactory recovery and precision (RSDs <20%) for all compounds at 10 ng/g and higher spiking levels, are aligned with the analytical quality control criteria of SANTE/12682/2019 guidelines. The cleanup effect of GCB was much superior to that of PSA, C18, and their combinations. The solvent exchange step with hexane was effective in removing co-extractives and minimizing matrix effects. Conclusions This method complies with the regulatory requirements and is fit-for-purpose for pesticide residue monitoring in turmeric. Highlights The study reports a validated GC-MS/MS method for multi-residue analysis of pesticides in turmeric for the first time. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision.

scholarly journals The Effect of Tanreqing Injection on the Pharmacokinetics of Sirolimus in Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Feng Zhang ◽  
Liang Sun ◽  
Jianxiu Zhai ◽  
Tianyi Xia ◽  
Wei Jiang ◽  
...  
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Matrix Effects ◽  
Thaw Cycle ◽  
Relative Standard ◽  
The Matrix ◽  
Freeze Thaw Cycle ◽  
Liquid Chromatography Tandem Mass ◽  
The Stability ◽  
First Time

To evaluate the effect of Tanreqing injection on the pharmacokinetics of sirolimus in rats, a high performance liquid chromatography tandem mass spectrometry method was developed for sirolimus assay in whole blood. Calibration curve of sirolimus was acquired over a concentration ranging from 2.5 to 100 ng/mL with r2= 0.9955. The matrix effects and extraction recoveries of sirolimus ranged from 144% to 152% and from 80% to 96%, respectively. The inter- and intraday relative standard deviations were both <10%. The stability investigation showed that the blood samples were stable for 30-day-storage at -20°C, for 8 h storage at room temperature, for 24 h storage in the auto-sampler at 4°C, and for three freeze-thaw cycle process. The pharmacokinetic results demonstrated that the Cmax, AUC, and AUMC of sirolimus in rats (7.5 mg/kg, i.g.) were increased after beincoadministration with Tanreqing Injection at 2.5, 5.0, and 7.5 mL/kg (i.v.), respectively, or at 5 min, 2 h, and 4 h (5.0 mL/kg, i.v.) after SRL dosing, respectively. For the first time, the results proved the herb-drug interaction between Tanreqing Injection and sirolimus and accordingly suggested avoiding concurrent reception of those two drugs for patients.

scholarly journals Optimized residue analysis method for broflanilide and its metabolites in agricultural produce using the QuEChERS method and LC-MS/MS

2020 ◽  
Author(s):  
Hyun Ho Noh ◽  
Chang Jo Kim ◽  
Hyeyoung Kwon ◽  
Danbi Kim ◽  
Byeong-chul Moon ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Residue Analysis ◽  
Brown Rice ◽  
Graphitized Carbon Black ◽  
Analysis Method ◽  
Preparation Methods ◽  
Green Pepper ◽  
Agricultural Produce ◽  
Liquid Chromatography Tandem Mass

AbstractSince broflanilide is a newly developed pesticide, analytical methods are required to determine the corresponding pesticide residues in diverse crops and foods. In this study, a pesticide residue analysis method was optimized for the detection and quantification of broflanilide and its two metabolites, DM-8007 and S(PFH-OH)-8007, in brown rice, soybean, apple, green pepper, mandarin, and kimchi cabbage. Residue samples were extracted from the produce using QuEChERS acetate and citrate buffering methods and were purified by dispersive solid-phase extraction (d-SPE) using six different adsorbent compositions with varying amounts of primary secondary amine (PSA), C18, and graphitized carbon black. All the sample preparation methods gave low-to-medium matrix effects, as confirmed by liquid chromatography–tandem mass spectrometry using standard solutions and matrix-matched standards. In particular, the use of the citrate buffering method, in combination with purification by d-SPE using 25 mg of PSA and a mixture of other adsorbents, consistently gave low matrix effects that in the range from −18.3 to 18.8%. Pesticide recoveries within the valid recovery range 70–120% were obtained both with and without d-SPE purification using 25 mg of PSA and other adsorbents. Thus, the developed residue analysis method is viable for the determination of broflanilide and its metabolites in various crops.

Fully-Automated SPE Coupled to UPLC-MS/MS Method for Simultaneous Detection of Trace Sulfonamides, Quinolones, and Macrolide antibiotics in Water

2021 ◽  
Author(s):  
Ming Zheng ◽  
Suwen Tang ◽  
Yangyang Bao ◽  
Kevin D Daniels ◽  
Zuo Tong How ◽  
...  
Keyword(s):  
High Performance ◽  
Matrix Effects ◽  
Solid Phase ◽  
Yangtze River Basin ◽  
Pure Water ◽  
Simultaneous Detection ◽  
Sample Volume ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract A fully automated solid-phase extraction (SPE) coupled ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for analysis of antibiotics (sulfonamides, quinolones, and macrolide) in water matrices. Sample preparation optimization included the selection of the best SPE material and configuration (HLB disks), sample volume (500−1000 mL water sample (pH = 3)) with a flow rate at 1−2 mL min− 1, and an elution procedure with 2 ⋅ 6 mL methanol, 2 ⋅ 6 mL acetone-methanol (V/V = 1/1). Meanwhile, the parameters for UPLC-MS/S detection of each analyte was optimized, including LC retention time, and MS parameters. The instrumental limits of detection (LOD) and quantification (LOQ) of analytes ranged from 0.01−0.72 µg L− 1 and 0.05−2.39 µg L− 1, respectively, with good linear correlation (R2 > 0.995) and precision (< 9.9%). Matrix spike recoveries ranged between 63.3−99.2% in pure water, 60.8−91.3% in surface water (SW), and 59.9−102.8% in wastewater effluent (WWE) with relative standard deviations (RSD) below 11%. The matrix effects (MEs) observed for most of the analytes were ion suppression (0−25.8%) except for four compounds that had enhancement (0−8.0 %) in SW or WWE. This method can basically meet the needs of trace antibiotic residues detection in waters. Trace levels of sulfonamides, quinolones and macrolides using the developed antibiotic method were below LOQ (BQL) −94.47 ng L− 1 in WWEs and BQL−15.47 ng L− 1 in SW in the lower reaches of the Yangtze River Basin.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

Optimization of thermal conductivity in composites loaded with the solid-solid phase-change materials

2018 ◽  
Vol 25 (6) ◽  
pp. 1157-1165
Author(s):  
Taoufik Mnasri ◽  
Adel Abbessi ◽  
Rached Ben Younes ◽  
Atef Mazioud
Keyword(s):  
Thermal Conductivity ◽  
Phase Change ◽  
Phase Change Materials ◽  
Solid Phase ◽  
Spherical Inclusions ◽  
First Case ◽  
The Matrix ◽  
Composite Conductivity ◽  
First Time

AbstractThis work focuses on identifying the thermal conductivity of composites loaded with phase-change materials (PCMs). Three configurations are studied: (1) the PCMs are divided into identical spherical inclusions arranged in one plane, (2) the PCMs are inserted into the matrix as a plate on the level of the same plane of arrangement, and (3) the PCMs are divided into identical spherical inclusions arranged periodically in the whole matrix. The percentage PCM/matrix is fixed for all cases. A comparison among the various situations is made for the first time, thus providing a new idea on how to insert PCMs into composite matrices. The results show that the composite conductivity is the most important consideration in the first case, precisely when the arrangement plane is parallel with the flux and diagonal to the entry face. In the present work, we are interested in exploring the solid-solid PCMs. The PCM polyurethane and a wood matrix are particularly studied.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

Synthesis of DABCO-based ionic liquid functionalized magnetic nanoparticles as a novel sorbent for the determination of cephalosporins in milk samples by dispersive solid-phase extraction followed by ultra-performance liquid chromatography-tandem mass spectrometry

2019 ◽  
Vol 43 (34) ◽  
pp. 13554-13570 ◽  
Author(s):  
Hamed Sahebi ◽  
Elaheh Konoz ◽  
Ali Ezabadi
Keyword(s):  
Ionic Liquid ◽  
Solid Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Dispersive Solid Phase Extraction ◽  
Magnetic Iron Oxide Nanoparticles ◽  
Chromatography Tandem Mass Spectrometry ◽  
Functionalized Magnetic Nanoparticles ◽  
Liquid Chromatography Tandem Mass ◽  
First Time

In this study, DABCO-based ionic liquid-functionalized magnetic iron oxide nanoparticles were synthesized for the first time by the quaternization reaction with 1-(2,3-dihydroxypropyl)-1,4-diazabicyclo[2.2.2]octanylium chloride and chloro-functionalized Fe3O4 nanoparticles.

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