Magnetic Solid-Phase Extraction Based on Amino-functionalized Magnetic Starch for Analysis of Organochlorine Pesticides

Abstract

A magnetic starch modified with 3,5-diaminobenzoic acid and 3aminopropyltriethoxysilane (Fe-starch@DABA-APTES) was synthesized and applied as adsorbent for extraction of organochlorine pesticides (OCPs). The magnetic solid-phase extraction was developed using 75 mg of the sorbent and 15 mL sample solution. Extraction was conducted on a vortex mixer for 40 s. The adsorbent was collected using an external magnet before eluting the analytes using 0.5 mL methanol. Quantification of the analytes was performed using gas chromatography with micro-electron capture detector. Linearity was obtained for the studied OCPs in the range between 0.01-2.00 g L -1 . The detection and quantification limits were obtained in the ranges of 0.5-4.0 and 1.5-15.0 ng L -1 , respectively, with the enrichment factors of up to 39.The precision in terms of intra-and inter-day relative standard deviations (RSDs) were below 4.75%, and 9.25%, respectively. The developed method has been applied in natural water and agricultural product samples. The recoveries ranged between 59.83-132.67% (RSDs<10.73%).

Review of scientific literature on available methods of assessing organochlorine pesticides in the environment

“…RT: 5.58–17.5 min” [ 301 ] Carrot, Onion, Cabbage, Garlic and Ginger 17 0.017–0.405 0.17–4.05 86.64–93.86 GC-ECD “initial oven temperature of 150 °C which was later increased to 280 °C at 6 °C/min and the total run time was 21.67 min. RT: 5.117–18.875 min” [ 302 ] Water, fruits and vegetable 7 0.0005–0.004 0.0015–0.015 Water: 69.61–121.95; veg: 59.83–132.67; fruit: 67.41–115.37 Water: <9.76; veg: 10.37; fruit: <10.03 GC-ECD: “Split, The oven temperature program was started at 160 °C for 0.5 min, raised to 180 °C at a rate of 20 °C min–1 and held for 0.5 min, raised to 190 °C at 20 °C min–1 and held for 0.5 min, raised to 250 °C at 40 °C min–1 and held for 4 min, and then to 300 °C at 25 °C min–1 and held for 2 min” [ 303 ] Tobacco leaves 20) 2–65.5 6.5 to 198 70–100 2.9–64.8 GC-ECD: “Splitless, the GC oven temperature was programmed as follows: 100C (0.5 min), 35C min1 to 220C, 10C min1 to 240C, 2C min1 to 250C, and 10C min1 to 290C (2 min). RT: 6.542–15.628” [ 304 ] Needle leaves 11 2.3 × 10 −4 -0.026 52–117 HRGC-HRMS: “The oven temperature was 60 °C initially, held for 1.5 min and ramped at 10 °C/min to 140 °C, then increased to 220 °C at 4 °C/min, and ramped at 2 °C/min to 250 °C, and finally ramped to 300 °C at 8 °C/min” [ 305 ] Pine needle 10 0–3.25 pg a ; IDL: 0.04 pg a 0–9.087 pg a 50–120 GC-MS: “initial temperature 50 °C (1min), 25 °C/min up to 200 °C, 8 °C/min up to 300 °C, 5.5 min stayed, 5 °C/min rise to 310 °C for 3 min” …”

Starch-Based Polymer Materials as Advanced Adsorbents for Sustainable Water Treatment: Current Status, Challenges, and Future Perspectives

“…In one study, a magnetic starch material, known as Fe-starch@DABA-APTES, was synthesized by modifying starch with 3,5-diaminobenzoic acid and 3-aminopropyltriethoxysilane. This magnetic starch material was then utilized as an adsorbent for the extraction of organochlorine pesticides (OCPs) [ 150 ].…”

Magnetic Polyeugenol Nanoparticles as a New Sorbent for Solid‐Phase Extraction of Polycyclic Aromatic Hydrocarbons in Environmental Water and Food Samples

“…So far, many biomagnetic adsorbents have been synthesized and used for SPE, [20,21] including: graphene oxide/chitosan composite, [22] biocharcoal aerogel sorbent, [23] greener monolithic based on calcium cross-linked starch cryogel composite graphene oxide nanoparticles, [24] magnetic peach gum polysaccharide, [25] magnetic curcumin, [26] magnetic cellulose, [27] agarose, [28] β-cyclodextrin functionalized graphene oxide [29] and functionalized magnetic starch. [30] Eugenol)C 10 H 12 O 2 ; phenylpropanoid (is a phenolic aromatic natural compound [31] that can be obtained from a variety of sources like clove oil, nutmeg oil, cinnamon bark and many other herbs. Eugenol is structurally composed of a benzene ring, allyl group, methoxy and hydroxyl groups.…”

“…Recently, bio‐sorbents have received much attention due to their compatibility with biological and environmental process, easy availability, simple and green synthesis procedure and low cost. So far, many biomagnetic adsorbents have been synthesized and used for SPE, [20,21] including: graphene oxide/chitosan composite, [22] biocharcoal aerogel sorbent, [23] greener monolithic based on calcium cross‐linked starch cryogel composite graphene oxide nanoparticles, [24] magnetic peach gum polysaccharide, [25] magnetic curcumin, [26] magnetic cellulose, [27] agarose, [28] β‐cyclodextrin functionalized graphene oxide [29] and functionalized magnetic starch [30] …”