scholarly journals Rapid Simultaneous Determination of 43 Pesticide Residues in Schizonepeta tenuifolia by Gas Chromatography Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Guo-wei Zhou ◽  
Yong-mei Li ◽  
Chun-ni Liu ◽  
Hong-min Ren ◽  
Hai-ying Li

A simple, fast, and reliable method was established for simultaneous determination of 43 pesticides in Schizonepeta tenuifolia. The samples were prepared using solid-phase extraction (SPE) method. Pesticides were extracted from Schizonepeta tenuifolia using acetonitrile, cleaned with Pesticarb/NH2, and eluted by mixed solvents of acetonitrile and toluene (3 : 1, v/v). Selected pesticides were identified using DB-35MS capillary column and detected by gas chromatography mass spectrometry. Samples were quantified by external standard method. Recoveries for the majority of pesticides at spike levels of 0.2, 0.5, and 1 mg kg−1 ranged between 70 and 120% (except for Chlorothalonil, Thiamethoxam, and Dicofol), and the relative standard deviations (RSDs n = 6) were 1.32%–13.91%. Limits of detection (LODs) were 0.0011–0.0135 mg kg−1, whereas limits of quantification (LOQs) were 0.0038–0.0451 mg kg−1. The satisfactory accuracy and precision, in combination with a good separation and few interferences, have demonstrated the strong potential of this technique for its application in Schizonepeta tenuifolia analysis.

2019 ◽  
Vol 9 (5) ◽  
pp. 879 ◽  
Author(s):  
Chien-Che Hung ◽  
Sailent Simaremare ◽  
Chia-Jung Hsieh ◽  
Lih-Ming Yiin

We have developed a rapid, sensitive, and reliable method for simultaneous determination of the urinary metabolites of common insecticides in a single analytical run using gas chromatography–mass spectrometry (GCMS). Thirteen metabolites, one originating from carbamate, six from organophosphates, and seven from pyrethroids, were selected for method validation. Samples at different concentrations (0.5–15 µg/L) were prepared by mixing working solutions containing the analytes with blank urine. After acid hydrolysis for 45 min at 90 °C, samples were processed with liquid–liquid extraction and derivatization by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA) before analysis on GCMS. The limits of detection for all thirteen analytes were below 0.1 µg/L. The recovery rates, evaluated at two concentrations (1, 10 µg/L), were found to be 90.48%, on average. The precision of multiple analyses at three different concentrations (0.5, 5, 15 µg/L) within one day or between 10 days was evaluated, and the resultant relative standard deviations were 8.1% or under. We also applied this method to analyze genuine urine samples collected from 30 human subjects, and successfully detected all the metabolites, with detection frequencies more than 50% for pyrethroid metabolites. In summary, this method is not only as good as others in performance, but is advantageous in terms of cost effectiveness and multiplicity of analytes.


2009 ◽  
Vol 63 (1) ◽  
Author(s):  
Xin Yang ◽  
De Xu ◽  
Jian Qiu ◽  
Hua Zhang ◽  
Ying Zhang ◽  
...  

AbstractAn efficient and sensitive method for simultaneous determination of 118 pesticide residues in teas has been established and validated. A multi-residue analysis of pesticides in tea involved extraction with ethyl acetate-hexane, clean-up using gel permeation chromatography (GPC) and solidphase extraction (SPE), and subsequent identification and quantification of the selected pesticides by gas chromatography-mass spectrometry (GC-MS). For most of the target analytes, optimized pretreatment processes led to no significant interference with analysis of sample matrix, and the determination of 118 compounds was achieved in about 60 min. In the linear range of each pesticide, the correlation coefficient was R 2 ≥ 0.99. At the low, medium and high three fortification levels of 0.05–2.5 mg kg−1, 118 pesticides average recoveries range from 61 % to 121 % and relative standard deviations (RSD) were in the range of 0.6–9.2 % for all analytes. The limits of detection for the method were 0.00030-0.36 mg kg−1, depending on each pesticide.


Author(s):  
Ha Binh Nguyen Thi ◽  
Cao Tien Bui ◽  
Ngoc Anh Mai Thi ◽  
Hoai Pham Thi ◽  
Hong Hao Le Thi ◽  
...  

A method for the simultaneous determination of furans, 2-methylfuran and 3-methylfuran in some food by gas chromatography-mass spectrometry (GC-MS) has successfully developed. Analysed samples were treated by a headspace technique using furan-d4 as an internal standard. The detection limit of the method is 0.3 µg/kg, the quantitative limit of the method is 1.0 µg/kg. The recovery of the method is in the range of 72 to 110%. The relative standard deviation ranges from 3.3 to 13%. The method was applied to analyze 100 food samples, including: coffees, canned meats, baby foods, powdered milk. The results showed that furans, 2-methylfuran, 3-methylfuran were detected in 30 samples out of 100 collected samples. In particular, furans were found in a ranges of 5.7 to 2803 µg/kg in all of coffee samples, including instant coffee and roasted coffee. In addition, furans were detected in one baby food sample contains, furans and 2-methylfuran in four canned meat samples, and no furans milk were detected in powder sample among 25 analysed samples.


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