The analytical standards of fipronil (purity of 97.9%) and its two metabolites desulfinyl (purity 97.8%) and sulfone (purity 99.7%) were purchased from Sigma-Aldrich, USA and the formulation of fipronil 5% SC (trade name: RULAR) was supplied by Krishi Rasayan Export Pvt. Ltd., New Delhi for field application in paddy. Ethyl acetate and acetonitrile (purity 99.9%, J.T. Baker, USA), millipore water (prepared from Milli-Q system, Millipore Corp., Billerica, MA), magnesium sulphate heptahydrate (ACS, Merck, India), sodium sulphate anhydrous (Merck, India), sodium acetate (SRL, India), acetic acid (Merck, India), primary secondary amine (PSA; 40 μm, Bondesil, Agilent, USA), C18 (ODS; Agilent, USA) and graphitized carbon black (GCB; UCT, Bellefonte, PA) were procured for use in residue analysis.
Bondesil
Manufactured by Agilent Technologies
Sourced in United States
Bondesil is a solid-phase extraction (SPE) product line offered by Agilent Technologies. Bondesil products are designed for sample preparation and purification applications in analytical chemistry. The Bondesil line includes a variety of sorbent materials and cartridge formats to accommodate different sample types and analytical needs.
Automatically generated - may contain errors
Lab products found in correlation
Sodium acetate, by Merck Group (1 mentions)
Anhydrous sodium sulphate, by Merck Group (1 mentions)
Milli q system, by Merck Group (1 mentions)
Ethyl acetate, by Avantor (1 mentions)
Acetonitrile, by Avantor (1 mentions)
Millipore water, by Merck Group (1 mentions)
Fipronil, by Merck Group (1 mentions)
Acetic acid, by Merck Group (1 mentions)
Milli q, by Merck Group (1 mentions)
Lc ms grade acetonitrile, by Merck Group (1 mentions)
Ammonium carbonate nh4 2co3, by Merck Group (1 mentions)
Class m10a, by Shimadzu (1 mentions)
3 protocols using bondesil
1
Fipronil and Metabolite Residue Analysis
2
Ergot Alkaloid Quantification Protocol
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Chemicals and solvents used for sample preparation were ‘pro-analysis’ quality or better. Milli-Q (Merk Millipore S.p.a, Milano, Italy) water was used. LC-MS grade acetonitrile (ACN) and ammonium carbonate (NH4)2CO3 were purchased from Sigma-Aldrich (Milano, Italy). Bondesil (Agilent Technologies, Santa Clara, CA, USA) Primary Secondary Amine (PSA) was used.
The analytical reference standards of ergometrine, ergosine, ergocornine, α-ergocryptine, ergotamine, ergocristine, ergometrinine, ergosinine, ergocorninine, α-ergocryptinine, ergotaminine, ergocristinine were purchased as dry film from Biopure (Tulln, Austria).
A standard mix solution was prepared in 100% ACN as a mix of all the EAs under examination at a concentration of 0.5 μg/mL of each of the alkaloids. This solution was diluted in ACN at 10 ng/mL to obtain a standard working solution used for preparation of calibration curves. All standard solutions were stored at −20 °C in amber vials.
The analytical reference standards of ergometrine, ergosine, ergocornine, α-ergocryptine, ergotamine, ergocristine, ergometrinine, ergosinine, ergocorninine, α-ergocryptinine, ergotaminine, ergocristinine were purchased as dry film from Biopure (Tulln, Austria).
A standard mix solution was prepared in 100% ACN as a mix of all the EAs under examination at a concentration of 0.5 μg/mL of each of the alkaloids. This solution was diluted in ACN at 10 ng/mL to obtain a standard working solution used for preparation of calibration curves. All standard solutions were stored at −20 °C in amber vials.
3
Phenolic Acid Profiling of Spirulina LEB-18
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Aliquots of 20 uL samples of phenolic extracts from Spirulina LEB-18 (diluted in water: methanol, 1:1) were injected into a chromatograph (Shimadzu, Tokyo, Japan, CLASS-M10A), flow 0.9 mL min -1 103 Kgf/ cm 2 at a temperature of 35 °C. The separation of the phenolic acids was accomplished using a C18 reverse phase column (4.6 × 250 mm, 5 μm; Bondesil, Agilent Technologies, CA, EUA) and an isocratic gradient of solvents consisting of methanol and acidified water (acetic acid 1%) in the ratio 20:80 v/v for 25 min, using detection at 280 nm to 320 nm and 15 min to 25 min. Phenolic acids were identified by comparison of retention times and absorption spectra with various standards such as caffeic, chlorogenic, ferulic, gallic, hydroxybenzoic, protocatechuic and vanillin as described in the literature (Pourali, Asghari, & Yoshida, 2010; Mira, Barros, Schiocchet, Noldin, & Lanfer-Marquez, 2008; . Zhou et al., 2004) . The limit of detection (LOD) was determined by the ratio of white noise signal (solution containing the solvent used in the extraction of phenolic compounds) of 3:1. The limit of quantification (LOQ) was established as being three times the LOD (Ribani, Bottoli, Collins, Jardim, & Melo, 2004) . The method was used according to Schmidt, Gonçalves, Prietto, Hackbart, and Furlong (2014) with modifications.
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