scholarly journals Development and Validation of GC-ECD Method for the Determination of Metamitron in Soil

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Shishir Tandon ◽  
Satyendra Kumar ◽  
N. K. Sand

This paper aims at developing and validating a convenient, rapid, and sensitive method for estimation of metamitron from soil samples.Determination andquantification was carried out by Gas Chromatography on microcapillary column with an Electron Capture Detector source. The compound was extracted from soil using methanol and cleanup by C-18 SPE. After optimization, the method was validated by evaluating the analytical curves, linearity, limits of detection, and quantification, precision (repeatability and intermediate precision), and accuracy (recovery). Recovery values ranged from 89 to 93.5% within 0.05- 2.0 µg L−1with average RSD 1.80%. The precision (repeatability) ranged from 1.7034 to 1.9144% and intermediate precision from 1.5685 to 2.1323%. Retention time was 6.3 minutes, and minimum detectable and quantifiable limits were 0.02 ng mL−1and 0.05 ng g−1, respectively. Good linearity (R2=0.998) of the calibration curves was obtained over the range from 0.05 to 2.0 µg L−1. Results indicated that the developed method is rapid and easy to perform, making it applicable for analysis in large pesticide monitoring programmes.

2019 ◽  
Vol 15 (1) ◽  
pp. 177
Author(s):  
Aman Sentosa Panggabean ◽  
Tika Widyastuti ◽  
Noor Hindryawati

<p>Penelitian tentang validasi metode penentuan kadar benzena, toluena dan xilena pada sampel udara dan tanah dengan menggunakan kromatografi gas telah dilakukan. Untuk mendapatkan hasil pengukuran yang valid, beberapa parameter penting yang berpengaruh dalam validasi metode telah ditentukan. Beberapa parameter penting yang dilakukan adalah penentuan besaran dasar kromatografi yang meliputi: waktu retensi, kapasitas (k’), faktor selektivitas (α) dan kinerja analitik yang meliputi: penentuan linearitas (r), limit deteksi (LOD), limit kuantitasi (LOQ), presisi dan akurasi. Hasil penelitian penentuan kinerja analitik sangat baik ditunjukkan oleh nilai presisi sebagai % KV &lt; 2/3 nilai KV Horwitz, LOD untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,02 mg/L; 0,59 mg/L dan 0,08 mg/L serta LOQ untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,07 mg/L; 1,99 mg/L dan 0,27 mg/L. Akurasi  metode ini sangat baik ditunjukkan dengan nilai presentase perolehan kembali masing-masing senyawa benzena, toluena dan xilena untuk sampel tanah sebesar 102,61 ± 4,61%; 101,65 ± 7,41%; 102,15 ± 4,15%, dan untuk sampel udara masing-masing senyawa sebesar 101,69 ± 5,77%; 102,08 ± 5,43% dan 98,55 ± 5,11%. Berdasarkan hasil penelitian ini, metode kromatografi gas dapat digunakan dalam penentuan benzena, toluena dan xilena pada sampel udara dan tanah dengan memberikan hasil yang valid.</p><p><strong>Validation Method </strong><strong>o</strong><strong>n The Determination </strong><strong>o</strong><strong>f Benzene, Toluene </strong><strong>a</strong><strong>nd Xylene </strong><strong>i</strong><strong>n Air </strong><strong>a</strong><strong>nd Soil Samples Using Gas Chromatography. </strong>The present study investigated the method for the determination of the content of benzene, toluene, and xylene in air and soil samples using gas chromatography. To obtain a valid measurement result, several important parameters that influence the method validation have been determined. The several important parameters carried out are the determination of the basic chromatographic such as retention time, capacity factor (k'), selectivity (α) and analytical performance measurement includes: the determination of linearity (r), limit of detection (LOD), limit of quantitation (LOQ), precision and accuracy. The result of analytical performance of the research are well verified, in which the value of precision was % CV &lt; 2/3 CV Horwitz value, LOD for benzene, toluene, and xylene compound were 0.02 mg/L, 0.59 mg/L, 0.08 mg/L, respectively, and LOQ for benzene, toluene and xylene compounds was 0.07 mg/L, 1.99 mg/L and 0.27 mg/L respectively. This method achieved high accuration, indicated by a percentage of recovery value of benzene, toluene, and xylene for soil samples of 102.61 ± 4.61%; 101.65 ± 7.41%; 102.15 ± 4.15%, and for air samples was 101.69 ± 5.77%, 102.08 ± 5.43%, and 98.55 ± 5.11% respectively. Based on the results of this research, the method presented in this study can be applied for the determination of benzene, toluene, and xylene using gas chromatography in air and soil samples with valid results.</p>


1963 ◽  
Vol 46 (2) ◽  
pp. 165-171
Author(s):  
A K Klein ◽  
J O Watts ◽  
J N Damico

Abstract The use of electron capture gas chromatography makes it possible to determine DDT in 1 g of butter and in 1 g of refined vegetable oils at the 0.1—1.0 ppm level of DDT. The precision is about 90%. The lowest limit for reliable measurements is 0.1 ppm DDT. At 0.05 ppm, DDT is not measured. A variable artifact, having the same retention time as p,p’-DDT, is the limiting factor. The presence of DDT may be confirmed by measuring and identifying DDE formed by alkaline hydrolysis.


1982 ◽  
Vol 237 (2) ◽  
pp. 285-292 ◽  
Author(s):  
Masaru Terada ◽  
Toshinori Yamamoto ◽  
Takemi Yoshida ◽  
Yukio Kuroiwa ◽  
Saburo Yoshimura

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