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Background: Angelica dahurica Radix and Osterici radix, are perennial herbs belonging to the family Umbelliferae, which were attacked by red spiders, thus fenpropathrin was registered. Fenpropathrin is important in improving productivity and quality of medicinal herbs due to timely pest control. However, residue may likely remain after harvest, and therefore, the residue analysis is important to ensure pesticides safety management. Objective: This study aimed to establish analysis method for fenpropathrin residues in A. dahurica Radix and O. radix using GLC-ECD and GC-MS/MS. Methods: Samples were moisturized with distilled-water and extracted with acetonitrile. The interferences were removed using SPE cartridges and analyzed by GLC-ECD and GC-MS/MS. Results: Based on pre-experiment results, the analysis method was optimized using double-cleanup method (SPE-GCB/NH2 & SPE silica cartridges). Fenpropathrin peak confirmed by GC-MS at the same retention time and with its mass numbers. Nevertheless, the cleanup processes are laborious and require a rather long time. Thus, additional effortless analysis method was developed using the d-SPE method that can apply to highly selective and sensitive GC-MS/MS. The LOD of GC-ECD and GC-MS/MS was 0.1 and 0.01 ng, respectively. While the LOQ was 0.04 mg/kg for both. Linearity (r2) was > 0.998 (GLC-ECD) and 0.999 (GC-MS/MS). The recoveries at three spiking levels ranged 83.6-103.1% and 89.6-98.0% for A. dahurica Radix and O. radix, respectively. Conclusion: Accuracy of the improved method met the standard of the Korean Ministry of Food and Drug Safety. Therefore, the developed methods expected to be used for analyzing pesticide residues in herbal medicines in Korea and other countries.
Background: Angelica dahurica Radix and Osterici radix, are perennial herbs belonging to the family Umbelliferae, which were attacked by red spiders, thus fenpropathrin was registered. Fenpropathrin is important in improving productivity and quality of medicinal herbs due to timely pest control. However, residue may likely remain after harvest, and therefore, the residue analysis is important to ensure pesticides safety management. Objective: This study aimed to establish analysis method for fenpropathrin residues in A. dahurica Radix and O. radix using GLC-ECD and GC-MS/MS. Methods: Samples were moisturized with distilled-water and extracted with acetonitrile. The interferences were removed using SPE cartridges and analyzed by GLC-ECD and GC-MS/MS. Results: Based on pre-experiment results, the analysis method was optimized using double-cleanup method (SPE-GCB/NH2 & SPE silica cartridges). Fenpropathrin peak confirmed by GC-MS at the same retention time and with its mass numbers. Nevertheless, the cleanup processes are laborious and require a rather long time. Thus, additional effortless analysis method was developed using the d-SPE method that can apply to highly selective and sensitive GC-MS/MS. The LOD of GC-ECD and GC-MS/MS was 0.1 and 0.01 ng, respectively. While the LOQ was 0.04 mg/kg for both. Linearity (r2) was > 0.998 (GLC-ECD) and 0.999 (GC-MS/MS). The recoveries at three spiking levels ranged 83.6-103.1% and 89.6-98.0% for A. dahurica Radix and O. radix, respectively. Conclusion: Accuracy of the improved method met the standard of the Korean Ministry of Food and Drug Safety. Therefore, the developed methods expected to be used for analyzing pesticide residues in herbal medicines in Korea and other countries.
Pesticide residue analysis in medicinal herbs is a challenging task because of the matrix effect and its influence on quantitative analysis despite the continuous development of several new analytical methods and instrumentations. In this study, a modified QuEChERS method was developed for the analysis of indoxacarb residue in medicinal herbs by using the conventional instrument, gas chromatography micro-electron-capture-detector (GC–μECD), and comparing it with gas chromatography–tandem mass spectrometry (GC–MS/MS) and liquid chromatography–tandem mass spectrometry (LC–MS/MS). Samples were extracted with acetonitrile and purified using an NH2 cartridge. The optimized method efficiently removes the co-extractives and offered a limit of quantification of 0.01 mg kg−1. The GC–μECD analysis results of indoxacarb in seven medicinal herbs out of fourteen species at a fortification level of 0.01 mg kg−1 showed a recovery range of 79.7–117.6%, while the rest showed recovery > 120%. Similarly, the recovery of indoxacarb by GC and LC–MS/SM were 74.1–105.9 and 73.0–99.0%, respectively, with a relative standard deviation of <20%. Matrix effects for the majority of medicinal herbs analyzed by GC–MS/MS were >±20%. Whereas the results for LC–MS/MS were <20%, which was within the acceptable range according to the SANTE/11312/2021 guidelines. Considering the performance of the method and alignment with the regulatory guidelines, LC–MS/MS is recommended for the analysis of indoxacarb in selected medicinal herbs.
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