scholarly journals An quantificational method for 51 pesticide residues determination in Pu'er tea by LC-MS/MS

Author(s):  
Xudong Wu ◽  
Zeyu Chen ◽  
Jiankang Zhang ◽  
Hongping Man ◽  
Tao Che ◽  
...  

<p>Pesticide residues in tea is a major issue due to their widely used in tea cultivation. Thus, to protect consumers, an appropriate method for determination of their residues in tea should be done. In this study, a method for the simultaneous determination of 51 pesticides in tea was developed and validated. The tea sample was extracted by acetonitrile and purified SPE clearnet TPT column followed by liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) with multi-reaction monitoring (MRM) mode. The method was validated according to the linearity, limit of detention, precision, the percentage of recovery at three different spike levels. The linear concentration range used was 10-100ng/ mL, the square of Correlation coefficient r2 was more than &gt;0.995. Recoveries were adequate being in the acceptable range of 72-89% and RSD of &lt;19 % for all the analytes at three level of 0.01,0.05 and 0.11mg/kg, the LOD of all chemicals from 0.001 mg/kg to 0.01 mg/kg .The method was applied for the determination for 400 tea samples collected from Pu'er which contain green tea and black tea. Among the analyzed samples , 36 % samples had Imidacloprid and 25% sample contain Acetamiprid, which were at a level below the European Union maximum residue levels (EU-MRLs). The information would be beneficial for Pu'er tea exporters.</p>

Mljekarstvo ◽  
2021 ◽  
Vol 71 (3) ◽  
pp. 165-174
Author(s):  
Milivoje Ćosić ◽  

Quality of milk plays a key role in its wide consumption but also of its involvement in a large series of derived products, such as yogurt, cheese, butter, and ice cream. An effective LC-MS/MS method has been validated for the determination of 81 different pesticide residues in milk samples. The analyses comprised 44 milk samples collected during 2019. From all inspected pesticides, only metalaxyl (present in 11.36 % samples), bifenthrin and metolachlor (9.09 %), dimethoate (4.55 %), prochloraz and thiacloprid were detected in 2.27 % of analysed samples. The detections of trifloxystrobin and bifenthrin were above the maximum residue levels (MRLs). The Commission Regulation (EU) 2017/1135 standardizes the MRLs for dimethoate and omethoate in certain products, but a MRL for dimethoate residues in milk has not been established jet. All the other pesticide detections were below the MRLs.


2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Heptachlor (14.60±3.60 µg L-1) and methoxychlor (12.60±2.20 µg L-1) showed dominant concentrations that were higher than 0.02 ng L-1 maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.


2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Heptachlor (14.60±3.60 µg L-1) and methoxychlor (12.60±2.20 µg L-1) showed dominant concentrations that were higher than 0.02 ng L-1 maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.


2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Hepachlor (14.60±3.60 µg/L) and methoxychlor (12.60±2.20 µg/L) showed dominant concentrations that were higher than 0.02 ng/L maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.


2012 ◽  
Vol 11 (1) ◽  
pp. 55-63 ◽  
Author(s):  
Maizbha Uddin Ahmed ◽  
Mohammad Safiqul Islam ◽  
Tasmin Ara Sultana ◽  
AGM Mostofa ◽  
Muhammad Shahdaat Bin Sayeed ◽  
...  

Azithromycin is an effective and well-known antimicrobial agent. In the present study, a simple, sensitive and specific LC/MS/MS method has been developed and validated for the quantification of Azithromycin in  human serum samples using Clarithromycin as internal standard. Azithromycin was extracted from biological matrix  by using solid phase extraction process. The chromatographic separation was performed on Luna C18 (3 ?, 2x150   mm) column with a mobile phase consisting of 35 mM ammonium acetate buffer (mobile phase-A) and acetonitrile  and methanol in ratio of 90:10 ( as mobile phase-B) at a flow rate of 0.25 mL/min. The method was validated over a  linear concentration range of 0.5?50.0 ng/mL and limit of quantification (LOQ) was 0.5 ng/mL with a coefficient of  correlation (r2) = 0.9998. The intra-day and inter-day precision expressed as relative standard deviation were 1.64% – 8.43% and 2.32% – 9.92%, respectively. The average recovery of azithromycin from serum was 98.11%. The method  was successfully applied to a pharmacokinetic study after oral administration of Azithromycin 200 mg/5 ml suspension in healthy Bangladeshi volunteers. DOI: http://dx.doi.org/10.3329/dujps.v11i1.12488 Dhaka Univ. J. Pharm. Sci. 11(1): 55-63, 2012 (June)


2001 ◽  
Vol 84 (6) ◽  
pp. 1927-1933 ◽  
Author(s):  
Stjepan Milardović ◽  
Zorana Grabarić ◽  
Vlatko Rumenjak ◽  
Nenad Blau ◽  
Dražen Milošević

Abstract This paper describes the performance of a biosensor with an Ru(III), Ni(II), and Fe(II) hexacyanometallate-modified graphite electrode and immobilized oxalate oxidase for the determination of urinary oxalate. The addition of ruthenium enhances the electrochemical reversibility and chemical stability of the electrocrystallized layer and improves the sensitivity of the biosensor. Hydrogen peroxide, produced by the enzyme-catalyzed oxidation of oxalate, was measured at −50 mV vs an Hg|Hg2Cl2|3M KCl electrode in a solution of pH 3.6 succinic buffer, 0.1M KCl, and 5.4mM ethylenediaminetetraacetic acid. The linear concentration range for the determination of oxalate was 0.18–280 μM. The recoveries of added oxalate (10–35 μM) from aqueous solution ranged from 99.5 to 101.7%, whereas from urine samples without oxalate (or with a concentration of oxalate below the detection limit) the recoveries of added oxalate ranged from 91.4 to 106.6%. The oxalate in 24 h urine samples, taken during their daily routine from 35 infants and children, was measured and found to range from 0.6 to 121.7 mg/L. There were no interferences from uric acid, acetylsalicylic acid, and urea in the concentration range investigated, but paracetamol and ascorbic acid did interfere. A good correlation (R2 = 0.9242) was found between values obtained for oxalate in real urine samples by 2 laboratories, with the proposed biosensor and ion chromatography, respectively.


2011 ◽  
Vol 94 (2) ◽  
pp. 634-644 ◽  
Author(s):  
Nikolaos G Tsiropoulos ◽  
Elpiniki G Amvrazi

Abstract A novel, simple, and rapid single-drop microextraction (SDME) procedure combined with GC has been developed, validated, and applied for the determination of multiclass pesticide residues in honey samples. The SDME was optimized using a Plackett-Burman screening design considering all parameters that may influence an SDME procedure and a consequent central composite design to control the parameters that were found to significantly influence the pesticide determination. The developed analytical method required minimal volumes of organic solvents and exhibited good analytical characteristics with enrichment factors ranging from 3 for -endosulfan to 10 for lindane, procymidone, and captan and method quantification limits ranging from 0.03 g/kg for phosalone to 10.6 g/kg for diazinon. The relative recoveries obtained ranged from 70.8 for captan to 120 for fenarimol, and the precision (RSD) ranged from 3 to 15. The proposed SDME procedure followed by GC with an electron capture detector for quantification and GC/MS for identification was applied with success to the analysis of 17 honey samples. Monitoring results indicated a low level of honey contamination by diazinon, chlorpyrifosethyl, procymidone, bromopropylate, and endosulfan (-, -, and endosulfan sulfate) residues that were far below the maximum residue limit values specified by the European Union for endosulfan (10 g/kg) and bromopropylate (100 g/kg) in honey samples.


2017 ◽  
Vol 80 (12) ◽  
pp. 2083-2089 ◽  
Author(s):  
Severine Koch ◽  
Astrid Epp ◽  
Mark Lohmann ◽  
Gaby-Fleur Böl

ABSTRACT Pesticide use and pesticide residues in foods have been the subject of controversial public discussions and media coverage in Germany. Against this background, a better understanding of public risk perceptions is needed to promote efficient public health communication. To this end, this study captures the German public's perception of pesticide residues in foods. A representative sample of the population aged 14 years and older (n = 1,004) was surveyed via computer-assisted telephone interviewing on their attitudes and knowledge with regard to pesticide residues. Based on questions regarding their typical consumer behavior, respondents were classified into conventional and organic consumers to identify differences as well as similarities between these two consumer types. As assessed with an open-ended question, both organic and conventional consumers viewed pesticides, chemicals, and toxins as the greatest threats to food quality and safety. Evaluating the risks and benefits of pesticide use, more than two-thirds of organic consumers (70%) rated the risks as greater than the benefits, compared with just over one-half of conventional consumers (53%). Concern about the detection of pesticide residues in the food chain and bodily fluids was significantly higher among organic compared with conventional consumers. Only a minority of respondents was aware that legal limits for pesticide residues (referred to as maximum residue levels) exist, with 69% of organic and 61% of conventional consumers believing that the presence of pesticide residues in foods is generally not permitted. A lack of awareness of maximum residue levels was associated with heightened levels of concern about pesticide residues. Finally, general exposure to media reporting on pesticide residues was associated with more frequent knowledge of legal limits for pesticide residues, whereas actively seeking information on pesticide residues was not. The possible mechanisms underlying these findings are discussed.


2012 ◽  
Vol 20 (2) ◽  
pp. 119-126 ◽  
Author(s):  
Magdalena Słowik-Borowiec ◽  
Ewa Szpyrka ◽  
Anna Kurdziel ◽  
Magdalena Grzegorzak ◽  
Aneta Matyaszek

Abstract During the 2010-2011 seasons, analyses of 171 samples of fresh fruit from the south-eastern region of Poland were performed. The research program included the determination of 137 (in 2010) to 152 (in 2011) active substances, together with their metabolites and decomposition products. The analytical methods used in the research were gas chromatography (GC/ECD/NPD) and spectrophotometry (to determine residues of dithiocarbamates). The results were compared with Poland’s allowed maximum residue levels (MRLs).Residues of active plant protection product substances were detected in 85 samples (50%), while 7 (4%) samples had exceeded the MRLs.Violations of MRLs were mainly concerned with the following group of insecticides: cypermethrin (in black currant), esfenwalerate (in raspberry), and the fungicides: propiconazole, and difenoconazole (in gooseberries).


Author(s):  
Turki Kh. Faraj Turki Kh. Faraj

A total of 81 samples of various leafy vegetables viz., Rocket (Eruca sativa), Lettuce (Lactuca sativa), Coriander (Coriandrum sativum), Corchorus (Corchorus olitorius), Parsley (Petroselinum crispum), Spinach (Spinacia oleracea), Radish (Raphanus sativus), Dill (Anethum graveolens), Mint (Mentha sachalinensis) and Green onions (Allium cepa) were collected from 20 different areas in Riyadh region of the Kingdom of Saudi Arabia. Liquid-Liquid Extraction of extraction partitioning method and confirmation by gas chromatograph-mass spectrometer for the presence of various pesticide residues was performed. Pesticide residues were detected in all the collected samples with varying concentrations. A variety of pesticides including organochlorines, organophosphates, pyrethroids, carbamates, herbicides, acaricides and insecticides have been identified in the samples. While the residue levels were low for most pesticides, higher levels of chlorpyrifos (0.123 mg/kg and resmethrin (0.1 mg/kg) were found in Rocket, carbaryl (0.92 mg/kg) in spinach and corchorus (0.116 mg/kg), permethrin (total cis + trans permethrin) inlettuce (0.103 mg/kg) and coriander (0.126 mg/kg), and cypermethrin in parsley (0.126 ppm). The highest maximum residue limit (MRL) values of pesticide residues on leafy vegetables of 0.10 mg/kg were observed for carbaryl in Spinach and Corchorus, whereas in Parsley an MRL of 0.5 mg/kg was found. The current research shows that in some leafy vegetables, higher doses of pesticides were found.


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