Research

12 pages, 1210 KiB

Open AccessArticle

Residues and Dietary Risk Assessment of Imidacloprid in Bamboo Shoot (Phyllostachys praecox), Winter Jujube (Ziziphus jujuba Mill. cv. Dongzao), Dendrobium officinale Kimura et Migo, and Fritillaria

by Yuan Lei, Yuqin Luo, Nan Fang, Yanjie Li, Xiangyun Wang, Hongmei He, Jinhua Jiang, Jianzhong Yu, Changpeng Zhang and Xueping Zhao

Agronomy 2023, 13(4), 1076; https://doi.org/10.3390/agronomy13041076 - 07 Apr 2023

Cited by 2 | Viewed by 1074

Abstract

The widespread use of pesticides poses significant risks to food and environmental safety. Imidacloprid is one of the most effective neuroactive neonicotinoid insecticides and is effective against a broad spectrum of piercing–sucking pests. A rapid, efficient, and high-throughput analysis method for the determination [...] Read more.

The widespread use of pesticides poses significant risks to food and environmental safety. Imidacloprid is one of the most effective neuroactive neonicotinoid insecticides and is effective against a broad spectrum of piercing–sucking pests. A rapid, efficient, and high-throughput analysis method for the determination of imidacloprid was developed in four minor crops with six matrices (bamboo shoot, winter jujube, fresh and dry D. officinale, and fresh and dry Fritillaria) by solid-phase extraction and HPLC-MS/MS. The procedure showed satisfying recoveries (72~111%) and RSDs (1~13%). A total of 288 samples were tested in China (Aba and Luan). Imidacloprid residues were 100% detected in fresh and dry D. officinale and winter jujube, with concentrations ranging from 0.048 to 1.550 mg·kg⁻¹. Imidacloprid residues were also abundant in fresh and dry Fritillaria (maximal concentration of 0.021 and 0.063 mg·kg⁻¹, respectively), followed by bamboo shoot, which had the lowest detection rate of imidacloprid (6%). Using the risk quotient (RQ) method, the long-term (RQ_c) and short-term (RQ_a) dietary risks of imidacloprid in bamboo shoot, winter jujube, fresh and dry D. officinale, and fresh and dry Fritillaria were further monitored. Based on the imidacloprid residues in this paper, the RQ_c and RQ_a were 15.03% and 0.0008~1.7604%, respectively. The RQ values were far less than 100%, showing that Chinese consumers face little health risk as a result of imidacloprid intake. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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9 pages, 261 KiB

Open AccessArticle

Residue Analysis and Dietary Risk Assessment of Metalaxyl in Chinese Bayberry and Dendrobium officinale

by Xiaomei Wang, Nan Fang, Xiangyun Wang, Yanjie Li, Jinhua Jiang, Yuqin Luo, Xueping Zhao, Changpeng Zhang and Qiang Wang

Agronomy 2023, 13(1), 186; https://doi.org/10.3390/agronomy13010186 - 06 Jan 2023

Cited by 3 | Viewed by 1300

Abstract

Metalaxyl is frequently used to protect a variety of crops from fungal diseases. This study aims to establish a method for the determination of metalaxyl in Chinese bayberry, fresh Dendrobium officinale (D. officinale), and dried D. officinale by gas chromatography-tandem mass [...] Read more.

Metalaxyl is frequently used to protect a variety of crops from fungal diseases. This study aims to establish a method for the determination of metalaxyl in Chinese bayberry, fresh Dendrobium officinale (D. officinale), and dried D. officinale by gas chromatography-tandem mass spectrometry (GC-MS/MS) and further assess dietary risk. The samples were extracted with acetonitrile and purified by the dispersed solid phase extraction method. Chinese bayberry, fresh D. officinale, and dried D. officinale samples were collected from Hangzhou and Zhangzhou in 2021 to clarify metalaxyl residue levels. The metalaxyl was quantitated by the external standard method. In the range of 0.001–0.1 mg L⁻¹, there was good linearity under the optimal conditions. The recoveries ranged from 83.90% to 110.47%, with relative standard deviations ranging from 0.86% to 5.81%. The detection rates in Chinese bayberry, fresh D. officinale, and dried D. officinale were 97.92%, 49.29%, and 50.71%, respectively. The dietary risk of metalaxyl residues in Chinese bayberry, fresh D. officinale, and dried D. officinale was acceptable for consumers. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

14 pages, 2300 KiB

Open AccessArticle

Dissipation, Residue, and Dietary Risk Assessment of Methoxyfenozide, Chlorantraniliprole, Indoxacarb, Lufenuron, and Chlorfenapyr in Spinach Using a Modified QuEChERS Method Combined with a Tandem Mass Spectrometry Technique

by Yizhi Feng, Guofu Zhang, Aijuan Zhang, Li Zhou, Yanli Bian, Jinju Pan, Sumei Yang, Jifeng Han, Xingang Ma, Xiaoxue Qi, Lin Liang and Bojun Zuo

Agronomy 2022, 12(12), 3173; https://doi.org/10.3390/agronomy12123173 - 15 Dec 2022

Cited by 2 | Viewed by 1612

Abstract

Spinach is a frequently consumed vegetable worldwide. Chemical pesticides are widely used to produce spinach with high yield and quality. However, the unregulated use of pesticides negatively impacts human and environmental health. A simple and efficient method using dispersive solid-phase extraction (d-SPE) combined [...] Read more.

Spinach is a frequently consumed vegetable worldwide. Chemical pesticides are widely used to produce spinach with high yield and quality. However, the unregulated use of pesticides negatively impacts human and environmental health. A simple and efficient method using dispersive solid-phase extraction (d-SPE) combined with field experiments was conducted to study the residue dissipation of methoxyfenozide, chlorantraniliprole, indoxacarb, lufenuron, and chlorfenapyr in spinach under different planting conditions. The results showed that the half-lives of methoxyfenozide, chlorantraniliprole, indoxacarb, lufenuron, and chlorfenapyr in spinach were 1.1–3.0 d, 2.6–4.0 d, 1.7–4.2 d, 3.4–4.4 d, and 2.8–4.3 d, respectively. The five pesticides rapidly degraded without significant differences between the open and greenhouse fields. The final residue of indoxacarb in spinach was not higher than the maximum residue limit (MRL) in China (3 mg kg⁻¹); the highest residual value was 1.0 mg kg⁻¹. Although the MRLs of methoxyfenozide, chlorfenapyr, and lufenuron for spinach are yet to be formulated in China, the long-term dietary risk for the four pesticides was acceptable, with an RQ < 100%, according to the international and national assessments. These results are necessary to provide guidance for the proper and safe use of these pesticides. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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12 pages, 979 KiB

Open AccessArticle

Dissipation and Dietary Risk Assessment of Thiacloprid and Tolfenpyrad in Tea in China

by Weitao Wang, Hongping Chen, Di Gao, Jiahuan Long, Hui Long and Ying Zhang

Agronomy 2022, 12(12), 3166; https://doi.org/10.3390/agronomy12123166 - 14 Dec 2022

Cited by 6 | Viewed by 1654

Abstract

Pesticides are widely used to maintain tea yields. For achieving satisfactory effects on pests, multiple pesticides in a low application dose have been the trend at present. In this study, we investigated the dissipation and dietary risk assessment of thiacloprid and tolfenpyrad. A [...] Read more.

Pesticides are widely used to maintain tea yields. For achieving satisfactory effects on pests, multiple pesticides in a low application dose have been the trend at present. In this study, we investigated the dissipation and dietary risk assessment of thiacloprid and tolfenpyrad. A method for the determination of thiacloprid and tolfenpyrad was developed. The recoveries ranged from 73% to 105% with standard deviations between 0.7% and 8.3%. Limits of quantification were 0.01 mg/kg for both pesticides. Field trials were conducted in China in 2021. The half-lives were in ranges of 3.22 to 8.45 days for thiacloprid and 2.91 to 10.50 days for tolfenpyrad. The terminal residues were in the range of 0.04–2.55 mg/kg for thiacloprid and <0.01–4.00 mg/kg for tolfenpyrad, respectively. Finally, a dietary risk assessment was conducted representing the acceptable risk of the two pesticides, which of ratios were all less than 100%. The safe pre-harvest interval of 14 days was suggested. This study can serve as a guide for the rational application of thiacloprid and tolfenpyrad in tea, which also ensures the safety of human health. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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22 pages, 5267 KiB

Open AccessArticle

TreeMerge: A Visual Comparative Analysis Method for Food Classification Tree in Pesticide Residue Maximum Limit Standards

by Zhiying Luo, Yi Chen, Hanqiang Li, Yue Li and Yandi Guo

Agronomy 2022, 12(12), 3148; https://doi.org/10.3390/agronomy12123148 - 12 Dec 2022

Cited by 4 | Viewed by 1477

Abstract

Food classification is an important part of food safety standards. In this paper, we propose a novel visual comparative analysis method for food classification trees (FCTs) in pesticide maximum residue limit (MRL) standards, called TreeMerge, to lay the foundation for a comprehensive comparison [...] Read more.

Food classification is an important part of food safety standards. In this paper, we propose a novel visual comparative analysis method for food classification trees (FCTs) in pesticide maximum residue limit (MRL) standards, called TreeMerge, to lay the foundation for a comprehensive comparison of pesticide MRL standards. First, a union tree is constructed by combining the two FCTs to be compared. Then, sunburst with an embedded chordal graph (SECG) and overlapping circular treemap (OCT), which are two new visualization solutions designed in this paper, are used to show the similarities and differences in a union tree. SECG can express the hierarchical structure and the similarity between corresponding nodes in the union tree at the same time. OCT uses an improved nested Venn diagram (overlapping circle) to express the attribute values in each layer of the union tree and uses a circle-filling layout algorithm based on the testing circle to improve the readability and space utilization of the view. Finally, a visual analysis system for comparing FCT, named FCTvis, is designed and implemented to support the exploration of the structural difference pattern of food classification in the two MRL standards and the quantity or scale of residue limits in various foods. The effectiveness of TreeMerge was verified by case studies on pesticide MRL standards in the Chinese Mainland and Chinese Hong Kong. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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11 pages, 1349 KiB

Open AccessArticle

Dissipation, Residue Behavior and Dietary Risk Assessment of Difenoconazole on Jujube (Ziziphus jujuba Mill.)

by Long Su, Jia Zhao, Chanjuan Liao, Han Wang, Sheng Xiong, Yaocheng Deng and Daoxin Gong

Agronomy 2022, 12(12), 3145; https://doi.org/10.3390/agronomy12123145 - 11 Dec 2022

Cited by 1 | Viewed by 1145

Abstract

Difenoconazole is a triazole germicide that is usually applied to prevent fungal diseases on crops with high efficiency and safety. Jujube is a spiny Rhamnaceous plant that originated in China more than 4000 years ago and is extensively cultivated in northern China nowadays. [...] Read more.

Difenoconazole is a triazole germicide that is usually applied to prevent fungal diseases on crops with high efficiency and safety. Jujube is a spiny Rhamnaceous plant that originated in China more than 4000 years ago and is extensively cultivated in northern China nowadays. To evaluate the safety of difenoconazole in jujube, supervised field trials were carried out in six provinces of China, and the final residue and dissipation behavior of difenoconazole on jujube were determined by gas chromatography (GC). The results showed that when addition levels were 0.02, 0.2, and 2 mg·kg⁻¹, average recoveries of the aforementioned method for difenoconazole in jujube can be put into the range of 73–108%, and relative standard deviation (RSD) was 3–9%. The limit of quantitation (LOQ) for this method was 0.02 mg·kg⁻¹. In the final residue test, difenoconazole was sprayed to deal with the jujube at 100 and 150 mg·kg⁻¹ doses twice or three times, respectively, while the dissipation test was applied only once at a 150 mg·kg⁻¹ dose. Final residue testing results have revealed that when jujube samples were harvested and tested at 7, 14, and 21 days post-application, difenoconazole residues in samples were 0.11–1.59, 0.05–0.77, 0.04–0.63 mg·kg⁻¹, respectively. The dissipation testing results showed that the digestion process of difenoconazole in jujube tends to be a gradual reduction process and the dynamic regularity of the residue dissipation proves consistent with the first-order dynamics reaction equation. The half-life (t_1/2) for difenoconazole residue dissipation in Qingdao and Yuncheng was 13.1 days and 16.5 days, respectively. The risk quotient (RQ) was 84.9% lower than 100%, showing that dietary intake risk to difenoconazole was acceptable and the maximum residue limit (MRL) of difenoconazole on jujube is recommended to be 2 mg·kg⁻¹. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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12 pages, 1959 KiB

Open AccessArticle

Assessment of Residuality of Hymexazol in Strawberry (Fragaria × ananassa) Crop by a Modified QuEChERS Method and Liquid Chromatography Tandem-Mass Spectrometry

by Manuel Alonzo Báez-Sañudo, Luis Alfonso Jiménez-Ortega and Pedro de Jesús Bastidas-Bastidas

Agronomy 2022, 12(12), 3110; https://doi.org/10.3390/agronomy12123110 - 08 Dec 2022

Viewed by 1469

Abstract

Hymexazol (HYM) is an active ingredient commonly used in a wide variety of crops; however, to date, there are no publications on its dissipation and residuality in strawberry fruits and leaves. The objective of the research was to evaluate the dissipation and residuality [...] Read more.

Hymexazol (HYM) is an active ingredient commonly used in a wide variety of crops; however, to date, there are no publications on its dissipation and residuality in strawberry fruits and leaves. The objective of the research was to evaluate the dissipation and residuality of hymexazol in strawberry using a modified QuEChERS method with UHPLC-ESI/MS-MS. For this, several validation experiments using the chromatographic method were conducted. The strawberry crop was established in the field, and the content of the HYM was monitored through several applications. The method showed good linearity (correlation coefficients > 0.9995), accuracy (recoveries in 73.7–109.4%), and sensitivity (limits of quantification 0.017 mg kg⁻¹). Despite the two and four drench-treatments of HYM in the strawberry crop, the compound was not detected at levels above the LOD 24 and 48 h after the last treatment. This is due to various plants metabolizing hymexazol to glucose conjugates of its tautomers, i.e., its O-glucoside and N-glucoside, probably with low or null movement to the aerial parts and fruits of the crop. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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9 pages, 1161 KiB

Open AccessArticle

Establishing the HPLC-MS/MS Method for Monitoring the Residue and Degradation of Butralin in Ginseng during Field and Risk Assessments

by Xiumei Wang, Qinghang You, Zhiguang Hou, Xiaolong Yu, Hemin Gao, Yuxue Gao, Liran Wang, Liping Wei and Zhongbin Lu

Agronomy 2022, 12(11), 2675; https://doi.org/10.3390/agronomy12112675 - 28 Oct 2022

Cited by 4 | Viewed by 1093

Abstract

Butralin can effectively mitigate the spreading of weeds in ginseng fields, however, the dissipation and residues of butralin in ginseng have not been investigated. In this study, we established a high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method to determine the butralin residue [...] Read more.

Butralin can effectively mitigate the spreading of weeds in ginseng fields, however, the dissipation and residues of butralin in ginseng have not been investigated. In this study, we established a high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method to determine the butralin residue and its dissipation in ginseng and its dietary intake risk. The mean recoveries of butralin in ginseng (fresh, dried, plants, and soil) ranged from 93.1–107.5% with relative standard deviations of 0.7–6.4%. The half-lives of butralin in ginseng plant and soil were 10.81–18.91 days, and its final residues in ginseng, dried gingeng, gingeng plant, and soil were <0.01, <0.010–0.02, 0.011–0.19, and 0.162–0.410 mg/kg, respectively. The dietary risk quotient of butralin was 3.25 × 10⁻⁴, which suggests that the consumption of butralin-treated ginseng during the harvest period does not affect human health. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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9 pages, 1167 KiB

Open AccessArticle

A Multi-Residue Method for the Determination of 77 Pesticides in Red Ginseng Using QuEChERS and Gas Chromatography/Tandem Mass Spectrometry (GC-MS/MS)

by Xuanwei Xu, Shuo Wang, Shengnan Hou, Ziqiang Li, Zhongbin Lu and Shuang Liang

Agronomy 2022, 12(10), 2479; https://doi.org/10.3390/agronomy12102479 - 12 Oct 2022

Cited by 5 | Viewed by 1617

Abstract

A simple, sensitive, and rapid multi-residue analytical method was developed based on gas chromatography-tandem mass spectrometry (GC–MS/MS) and used to determine 77 multiclass pesticides in red ginseng. Samples were extracted and purified via a modified QuEChERS method. The calibration curves were in the [...] Read more.

A simple, sensitive, and rapid multi-residue analytical method was developed based on gas chromatography-tandem mass spectrometry (GC–MS/MS) and used to determine 77 multiclass pesticides in red ginseng. Samples were extracted and purified via a modified QuEChERS method. The calibration curves were in the range of 5 to 200 ng mL⁻¹. The limits of detection (LODs) of the method were from 0.08 to 4.0 μg kg⁻¹ and limits of quantification (LOQs) were in the range of 0.2–12.0 μg kg⁻¹. The average recoveries of the method ranged from 61% to 133.9% at two spiked levels of 20 and 100 μg kg⁻¹ in red ginseng samples, with relative standard deviations (RSDs) of 0.2% to 14.9%. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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14 pages, 2848 KiB

Open AccessArticle

Establishment of a QuEChERS-UPLC-MS/MS Method for Simultaneously Detecting Tolfenpyrad and Its Metabolites in Tea

by Zihan Wang, Xinru Wang, Min Wang, Ziqiang Li, Xinzhong Zhang, Li Zhou, Hezhi Sun, Mei Yang, Zhengyun Lou, Zongmao Chen and Fengjian Luo

Agronomy 2022, 12(10), 2324; https://doi.org/10.3390/agronomy12102324 - 27 Sep 2022

Cited by 4 | Viewed by 1358

Abstract

An analytical method simultaneously detecting pesticide and its metabolites, especially with higher toxicity, was urgently needed for supervision and safety evaluation of agricultural products. In the present study, a modified QuEChERS method coupled with a ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for [...] Read more.

An analytical method simultaneously detecting pesticide and its metabolites, especially with higher toxicity, was urgently needed for supervision and safety evaluation of agricultural products. In the present study, a modified QuEChERS method coupled with a ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for simultaneous determination of tolfenpyrad (TFP) and its metabolites in tea matrices (fresh tea shoots, green tea, black tea, green tea infusion and black tea infusion) was established. The method validation showed good linearity (correlation coefficients ≥ 0.9945), accuracy (recoveries in 75.38–109.90%), sensitivity (limits of quantification ≤ 0.05 mg kg⁻¹), and precision (relative standard deviations ≤ 19.09%). The established method was then applied to detect 40 market samples, resulting in 60.0% positive rate of TFP, besides, two metabolites including PT-CA, which is more toxic than the parent TFP, and PT-OH were also detected in the samples with high TFP residue (≥0.048 mg kg⁻¹). The method established in the present work was thus of significant importance in comprehensive monitoring and of TFP in tea products. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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14 pages, 1480 KiB

Open AccessArticle

The Green Manure (Astragalus sinicus L.) Improved Rice Yield and Quality and Changed Soil Microbial Communities of Rice in the Karst Mountains Area

by Fang Wang, Honghao Cui, Fangwei He, Qian Liu, Qing Zhu, Wenhua Wang, Heng Liao, Danjun Yao, Weidong Cao and Ping Lu

Agronomy 2022, 12(8), 1851; https://doi.org/10.3390/agronomy12081851 - 04 Aug 2022

Cited by 6 | Viewed by 1771

Abstract

The use of green manure plants for soil restoration is a viable agricultural practice that can mitigate soil degradation and biodiversity loss caused by the long-term application of inorganic fertilizers. However, the effects of green manure on soil microbial communities, rice yield, and [...] Read more.

The use of green manure plants for soil restoration is a viable agricultural practice that can mitigate soil degradation and biodiversity loss caused by the long-term application of inorganic fertilizers. However, the effects of green manure on soil microbial communities, rice yield, and quality in the karst mountains are largely unknown. The effects of no chemical fertilizer, chemical fertilizer, chemical fertilizer + different Astragalus sinicus L. (Chinese milk vetch, CMV) treatments on the microbial community, soil enzyme activities, soil nutrient content, and crop yield were investigated through field experiments. A moderate application of chemical fertilizer with green manure can increase chlorophyll content, increase effective rice spikes, positive impact on rice yield, and increase crude protein, etc. Additional application of the moderate amount of CMV can increase alkali-hydrolyzable nitrogen and available phosphorus (a significant increase of 54.87–72.65%), improve microbial biomass carbon (MBC) and microbial biomass nitrogen (MBN) (CFMV2 significantly increased by 22.16%), improve soil urease and phosphatase activities, and the urease activity increased by 43.43–69.24% with CMV application compared to CK. Moreover, all bacterial communities were dominated by three major phyla (Proteobacteria, Chloroflexi, and Acidobacteria), where the application of chemical fertilizer with CMV increased the ratio of abundance of Proteobacteria and Acidobacteria in rice soils, and the effect of chemical fertilizer application on the dominant bacteria was regulated to some extent by additional green manure application, which may have a beneficial effect on rice yield. Therefore, we conclude that the rational use of chemical fertilizers with CMV (22,500 kg ha⁻¹) in karst landscapes is one of the effective measures to achieve efficient and sustainable use of rice fields. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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15 pages, 1260 KiB

Open AccessArticle

Simultaneous Quantitative Determination of Residues of Pyriproxyfen and Its Metabolites in Tea and Tea Infusion Using Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry

by Hongxia Li, Qing Zhong, Xinru Wang, Fengjian Luo, Li Zhou, Zongmao Chen and Xinzhong Zhang

Agronomy 2022, 12(8), 1829; https://doi.org/10.3390/agronomy12081829 - 01 Aug 2022

Cited by 6 | Viewed by 1484

Abstract

A reliable, simultaneous residue-analysis method for pyriproxyfen and its five metabolites in fresh tea leaves, green tea, black tea, green-tea infusion and black-tea infusion was developed and validated. The samples were extracted with acetonitrile, purified using a modified QuEChERs (quick, easy, cheap, effective, [...] Read more.

A reliable, simultaneous residue-analysis method for pyriproxyfen and its five metabolites in fresh tea leaves, green tea, black tea, green-tea infusion and black-tea infusion was developed and validated. The samples were extracted with acetonitrile, purified using a modified QuEChERs (quick, easy, cheap, effective, rugged and safe) method and determined using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). The method was successfully calibrated in the range of 0.005–2.50 mg/L with correlation coefficients (r) equal to or above 0.9957. The limits of detection (LODs) were less than 0.002 mg/L. The average spiked recoveries of pyriproxyfen and its metabolites at four levels were 71.2~102.9% with relative standard deviations (RSDs) of 0.3~14.4%. The limits of quantification (LOQs) in fresh tea leaves, tea and tea infusion were 0.002 mg/kg, 0.005 mg/kg and 0.0002 mg/L, respectively. This proposed method was feasible and was applied to analyze the residues of pyriproxyfen and its five metabolites on real fresh tea leaf samples. The results indicated that the half-life (t_1/2) of pyriproxyfen on fresh tea leaves was 2.48 d, and the five metabolites were detected on fresh tea leaves during field growth after application. Full article

(This article belongs to the Special Issue Pesticide Residues and Nutritional Quality of Agro-Products)

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