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.

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.

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.

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.

Determination of Imidacloprid, Acetamiprid, Thiabendazole and Carbendazim Residues in Edible Fungi by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 99-103 ◽  
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Zheng Peng ◽  
Ming Yue Wang ◽  
Zong Qiang Zeng ◽  
...  
Keyword(s):  
Solid Phase ◽  
Residue Analysis ◽  
Correlation Coefficients ◽  
Edible Fungi ◽  
Extraction Solvent ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Straw Mushroom

A method was developed for simultaneous determination of imidacloprid,acetamiprid, thiabendazole and carbendazim in lentinus edodes, straw mushroom and oyster mushroom by HPLC. Acetonitrile was edded in the sample for extraction solvent, the sample was purified by NH2 solid phase extraction cartridge,then detected by HPLC.The results showed that a good linearity in the range of 0.05~5.0μg/mL with the linear correlation coefficients of 0.9991~0.9997, the detection limits of imidacloprid, acetamiprid, thiabendazole and carbendazim were respectively 0.002 mg/kg,0.005mg/kg, 0.003 mg/kg and 0.003 mg/kg.Tests for recovery were made by addition of four pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates were 86.0%~105.0% , the relative standard deviations were less than 3.5%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

scholarly journals In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection

2017 ◽  
Vol 38 (6) ◽  
pp. 3539 ◽  
Author(s):  
Carolina Kato Prado ◽  
Flavio Dias Ferreira ◽  
Erika Bando ◽  
Miguel Machinski Junior
Keyword(s):  
Solid Phase ◽  
Residue Analysis ◽  
Cow Milk ◽  
Effective Control ◽  
Gradient System ◽  
Detection Capability ◽  
Reverse Phase ◽  
Accuracy And Precision ◽  
Tetracycline Residues ◽  
Maximum Limit

The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.

Determination of Tetracyclines Residues in Aquatic Products by HPLC

2014 ◽  
Vol 1004-1005 ◽  
pp. 914-918 ◽  
Author(s):  
Ling Lin ◽  
Hong Bin Guo ◽  
Qi Li ◽  
Li Qiang Zhang ◽  
Li Li Liu ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Residue Analysis ◽  
Pesticide Residue Analysis ◽  
Aquatic Products ◽  
Buffer Solutions ◽  
Aquatic Product ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision

A sensitive method for simultaneously determining residues of oxytetracycline, tetracycline ,chlortetracycline and doxycycline in aquatic product was established by HPLC. Samples were extracted with Na2EDTA-Mcllvaine buffer solutions and centrifuged.The sample extracts were cleaned up by C18 solid-phase extraction cartridge and then were determined by UV detection at 355 nm.At fortification levels of 0.005~0.1 mg/kg, the average recoveries were of 75%~96% , The RSDs were of 1.02%~6.56%,Limit of detection was 0.002 mg /kg for oxytetracycline,tetracycline and doxycycline and 0.005 mg /kg for chlortetracycline.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

Determination of Imidacloprid, Carbendazim and Thiabendazole Residues in Vegetables and Fruits by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 1392-1396 ◽  
Author(s):  
Ling Lin ◽  
Zheng Peng ◽  
Chun Liang Yang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  
Keyword(s):  
Fruits And Vegetables ◽  
Solid Phase ◽  
Residue Analysis ◽  
Extraction Solvent ◽  
Solid Phase Extraction Cartridge ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Vegetables And Fruits ◽  
Concentration Levels

The aim of this work was to establish a method that the residues of imidacloprid,carben-dazim and thiabendazole in fruits and vegetables were determined by HPLC.Acetonitrile was edded in the sample for extraction solvent, and using sodium chloride for absorbing water of the sample,then purified by NH2 solid phase extraction cartridge, the sample was detected by HPLC.Under the selected conditions,the detection limits of imidacloprid, carbendazim, thiabendazole were 0.002 mg/kg,0.003 mg/kg and 0.003 mg/kg respectively.Tests for recovery were made by addition of three pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates of imidacloprid, carbendazimand thiabendazole were87.0%~99.2%,82.0%~96.0% and 80.0%~95.0% respectively , and the relative standard deviations were 0.52%~6.80%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

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