• Journal of the Korean Society of International Agriculture
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• v.30 no.4
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• pp.339-346
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• 2018

Cyanazine is a member of the triazine family of herbicides. Cyanazine is used as a pre- and post-emergence herbicide for the control of annual grasses and broadleaf weeds. This experiment was conducted to establish a determination method for cyanazine, as domestic unregistered pesticide, residue in major agricultural commodities using HPLC-DAD/MS. Cyanazine was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and partitioned to dichloromethane for remove polar extractive in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. On a $C_{18}$ column in HPLC, cyanazine was successfully separated from co-extractives of sample, and sensitively quantitated by diode array detection at 220 nm. Accuracy and precision of the proposed method was validated by the recovery experiment on every major agricultural commodity samples fortified with cyanazine at 3 concentration levels per agricultural commodity in each triplication. Mean recoveries were ranged from 83.6 to 93.3% in five major representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring(SIM) technique was also provided to clearly identify the suspected residue.

• Korean Journal of Medicinal Crop Science
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• v.24 no.3
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• pp.237-245
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• 2016

Background: Cyanazine is used as a pre-emergent herbicide once during the growing season to control weeds of many upland crops worldwide. This study aimed to establish a method to determined cyanazine residue levels in major medicinal crops by using high performance liquid chromatography-UV detection/mass spectometry (HPLC-UVD/MS). Methods and Results: Cyanazine residue was extracted with acetone from the raw products of four representative medicinal plants - Scutellaria baicalensis, Paeonia lactiflora, Platycodon grandiflorum and Angelica gigas. The extract was diluted with a large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. It was then purifined using optimized Florisil column chromatography. HPLC analysis conducted using an octadecylsilyl column allowed the successful separation of cyanazine from co-extractives of the samples, and the amount was sensitively quantified by ultraviolet absorption at 225 nm with no interference. The accuracy and precision of the proposed method were validated by conducting recovery experiments on each medicinal crop sample fortified with cyanazine at two concentration levels per crop in triplicate. Conclusions: The mean recoveries ranged from 91.2% to 105.3% for the four representative medicinal crops. The coefficients of variation were less than 10%, irrespective of the sample types and fortification levels. The limit of quantification of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method was performed by liquid chromatography/MS using selected-ion monitoring technique to clearly identify the suspected residue.

• Journal of Food Hygiene and Safety
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• v.36 no.1
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• pp.1-8
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• 2021

The inverted Y-shaped strip detection method based on acetylcholinesterase (AChE) was developed for the rapid detection of organophosphorus and carbamate pesticides. The inactivation of AChE by organophosphorus and carbamate pesticides has been well known. The AChE catalyzes acetylthiocholine into thiocholine having (-) and (+) charges, and the (+) charge results in aggregation of gold nanoparticle (GNP). Malaoxon and carbofuran were used as standard organophosphorus and carbamate for the development of the inverted Y-shaped strip, respectively. In order to optimize the method, various angles of the Y-shaped strip, different types of nitrocellulose membrane, and concentration of AChE were tested as key parameters. The detection limit of the method was 10 ng/mL for both malaoxon and carbofuran pesticides. No cross-reaction was observed to other pesticides such as atrazine, cyanazine, simazine, bifenthrin, boscalid, metalaxyl, and chlorobenzilate. Recoveries from lettuce spiked when known concentrations of malaoxon and carbofuran were found ranging from 96.4 to 100.7% and 81 to 112.7%, respectively. This study suggests that the inverted Y-shaped strip method based on AChE may be a useful tool for the sensitive, specific, rapid detection of organophosphorus and carbamate pesticides in agricultural products.