超高效液相色谱-串联质谱法测定水稻基质中阿维菌素残留量

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定水稻基质中阿维菌素残留量,考察了基质效应,并对实际样品进行了检测.稻田土、稻壳、糙米和稻杆经乙腈振荡提取,稻田水经乙酸乙酯液液分配提取后,用C18固相萃取小柱或弗罗里硅土柱净化,采用UPLC-MS/MS正离子扫描测定残留的阿维菌素.稻田土、稻田水和糙米的3种添加浓度(1.0,10.0和100 μg/kg或μg/L)的平均回收率为84％～107％,相对标准偏差为4.7％～13.6％.稻壳和稻杆的2档添加浓度(10.0和100 μg/kg)的平均回收率为90％和103％,相对标准偏差为8.4％～12.9％.本方法在稻田水、糙米和稻田土中的检出限为0.3μg/kg在稻壳和稻杆中检出限为3.0 μg/kg,低于欧盟和日本在稻米中制定的阿维菌素最大残留限量值.阿维菌素在2.0～100 μg/L范围内线性关系良好( r＞ 0.999).     

Determination of RH‐5849 and indoxacarb in rice straw,rice husk,brown rice and soil using liquid chromatography–tandem triple quadrupole mass spectrometry following extraction with QuEChERS method

A fast and simple analytical method was developed for the simultaneous determination of RH‐5849 and indoxacarb in soil, rice straw, rice husk and brown rice. QuEChERS (quick, easy, cheap, effective, rugged and safe) method was used for extraction, and liquid chromatography with tandem triple quadrupole mass spectrometry was used for quantification. The matrix‐matched calibration plots were linear in the range between 25 and 5000 μg/L for soil, rice straw, rice husk and brown rice samples. All determination coefficients (R²) were ≥0.9962. The limits of detection and quantification were 1.5 and 5 μg/kg, respectively. Recoveries at three fortification levels ranged between 79.5 and 97.9% with relative standard deviations <11%. The developed method was validated and applied for the analysis of dissipation study samples. For field experiments, the half‐lives of RH‐5849 and indoxacarb in rice straw were 11.93 and 5.83 days, respectively. The method was demonstrated to be reliable for the routine monitoring of RH‐5849 and indoxacarb in rice samples. Copyright © 2016 John Wiley & Sons, Ltd.     

Simultaneous determination of sulfoxaflor and its metabolites,X11719474 and X11721061, in brown rice and rice straw after field application using LC-MS/MS

The present study was carried out to develop an analytical method for simultaneously detecting and quantifying sulfoxaflor and its metabolites (X11721061, X11719474) in brown rice and rice straw using liquid chromatography–tandem mass spectrometry. The parent compound and its metabolites were extracted and purified using original ‘QuEChERS’ method with modification. The matrix-matched calibration curve of sulfoxaflor and its metabolites in both matrices achieved good linearity with determination coefficients (R²) ≥0.9944. The overall recoveries of sulfoxaflor at two fortification levels (rice: 0.2 and 1.0 mg/kg; rice straw: 0.4 and 2.0 mg/kg) ranged from 97.37% to 107.71% with relative standard deviations (RSDs) <5%. On the other hand, the recoveries of both metabolites (X11721061 and X11719474) at 0.1 and 0.5 mg/kg (rice) and 0.2 and 1.0 mg/kg (rice straw) were satisfactory with values ranging from 83.70 % to 112.60% with RSDs <8%. During storage at ?20°C, the analyte and its metabolites were stable for up to 87 days. The limits of quantification of 0.02 mg/kg were lower than the maximum residue limit (0.2 mg/kg) set by the Korean Ministry of Food and Drug Safety for brown rice. The method was successfully applied to paddy field treated with different programme schedules and a preharvest interval of 7 days was proposed based upon the current study. In sum, the developed method is accurate and reproducible for ensuring the reliable determination of sulfoxaflor (and its metabolites) in harvested rice grain and straw samples from the field. The residual level of parent compound does not seem to pose any hazardous effect and treated rice could be safely used for consumption.     

Residues and dissipation of guadipyr in rice ecological system

A modified QuEChERs method with liquid chromatography-tandem mass spectrometry for analysis of guadipyr residue and dissipation in rice matrices, paddy soil and paddy water was developed and validated. Mean recoveries and relative standard deviations in paddy soil, paddy water, rice plant, rice straw, rice hull and husked rice matrices at three spiking levels were 83.1–116.5% and 1.6–9.5%, respectively. The half-life of guadipyr was determined in 2 years at three different field sites in China via a dissipation experiment. The half-lives of guadipyr in paddy water were 0.22–0.37 days, 0.24–3.33 days in paddy soil and 0.44–1.90 days in rice plant. The terminal residues of guadipyr ranged from ND (concentrations of guadipyr were below limit of detection) to 50 μg kg^?1 in paddy soil, 10–470 μg kg^?1 in rice hull, ND70 μg kg^?1 in husked rice and ND to 110 μg kg^?1 in rice straw. The results would be helpful in fixing maximum residue limit of guadipyr, a new insecticide, in rice.     

Dissipation dynamics of fenoxaprop-p-ethyl and fenoxaprop acid under Indian rice field conditions

Dissipation dynamics of fenoxaprop-p-ethyl (FPPE) and fenoxaprop acid (FPA) (metabolite) in rice field conditions was investigated for two consecutive seasons. FPPE dissipated rapidly in soil with average half life of 1.42–2.19 days. Dissipation followed first-order kinetics. The method was validated in terms of accuracy, linearity, specificity and precision. Linearity was in the range of 0.005–5 µg mL^?1 with limit of detection as 0.002 and 0.001 µg mL^?1 for fenoxaprop-p-ethyl and fenoxaprop acid, respectively. Quantitation limit in soil, grain, straw and husk were 0.005, 0.008, 0.01 and 0.01 µg g^?1 for fenoxaprop-p-ethyl, and 0.005, 0.01, 0.01 and 0.01 µg g^?1 for fenoxaprop acid, respectively. Recovery in soil, rice grains, straw and husk ranged from 81.60–93.40, 77.85–87.00, 75.20–84.40 and 76.00–87.20% for FPPE and 82.50–88.20, 76.25–83.00, 74.80–83.60 and 75.00–85.40% for FPA, respectively. Below detectable limit of residues of FPPE and metabolite were observed in soil, rice grain, husk and straw samples at harvest. FPPE and FPA were of short persistence under field conditions and residues were below European Union-Maximum Residue Limits in all matrices that would cause adverse effect on environment and human/animal health.     

高效液相色谱法分析水稻和稻田中的氯硝柳胺乙醇胺盐残留

建立了高效液相色谱(HPLC)测定水稻和稻田中氯硝柳胺乙醇胺盐残留量的分析方法。稻田水和稻秆样品中的氯硝柳胺乙醇胺盐残留用碱性乙酸乙酯直接提取;而稻田土壤、糙米和谷壳样品则先经碱性乙醇提取,再用乙酸乙酯进行萃取。萃取物经弗罗里硅土柱净化后,经Welchrom C18柱分离,采用紫外检测器检测,外标法定量。在0.01～10.00 mg/L范围内,氯硝柳胺乙醇胺盐的峰面积与其质量浓度间呈良好的线性关系,相关系数为0.9998。在稻田水、土壤、稻秆、糙米和谷壳中添加0.01～5.00 mg/kg的氯硝柳胺乙醇胺盐,其平均回收率为93.47%～100.9%,相对标准偏差为1.46%～5.82%,符合农药残留量分析与检测的技术要求。该方法简便、快速,灵敏度高,重现性好,可用于环境系统中氯硝柳胺乙醇胺盐残留量的分析与检测。     

Determination,residue and risk assessment of trifloxystrobin,trifloxystrobin acid and tebuconazole in Chinese rice consumption

A simple and rapid analytical method for the detection of trifloxystrobin, trifloxystrobin acid and tebuconazole in soil, brown rice, paddy plants and rice hulls was established and validated by liquid chromatography with tandem mass spectrometry. Acceptable linearity (R² > 0.99), accuracy (average recoveries of 74.3–108.5%) and precision (intra- and inter-day relative standard deviations of 0.9–8.8%) were obtained using the developed determination approach. In the field trial, the half-lives of trifloxystrobin and tebuconazole in paddy plants were 5.7–8.3 days in three locations throughout China, and the terminal residue concentrations of trifloxystrobin and tebuconazole were <100 and 500 μg/kg (maximum residue limits set by China), respectively, at harvest, which indicated that, based on the recommended application procedure, trifloxystrobin and tebuconazole are safe for use on rice. The risk assessment results demonstrated that, owing to risk quotient values of both fungicides being <100%, the potential risk of trifloxystrobin and tebuconazole on rice was acceptable for Chinese consumers. These data could provide supporting information for the proper use and safety evaluation of trifloxystrobin and tebuconazole in rice.     

Analysis of Enestroburin Residues in Wheat and Soil by Solid Phase Extraction and High-Performance Liquid Chromatography

A method was developed for the determination of enestroburin residues in wheat grain, wheat straw, and soil by solid-phase extraction (SPE) and HPLC-UV. The analytes were extracted with acetonitrile, cleaned up by PestiCarb/NH₂ cartridges and determined by HPLC with UV detector. This method is characterized by recovery >88.0%, precision (RSD) <7.8% and sensitivity of 0.005 mg/kg, in agreement with directives for method validation in residue analysis. The proposed method was successfully employed for the determination of enestroburin residue levels and its dissipation rates in a field trial in Beijing, China. Dissipation study shows that the half life of enestroburin in wheat straw was 5.35–5.81 days and in soil was 6.13–6.75 days. When enestroburin was applied according to the recommended dose and doubled dose, the final residue in wheat grain was both lower than 0.2 mg/kg. A harvest interval should be more than 7 d, and a dosage of 100–200 g (a.i.)/ha was suggested and considered as safe to human beings and animals.     

Dissipation and residue of flonicamid in cucumber,apple and soil under field conditions

A method based on QuEChERS-like extraction and UPLC-ESI-MS/MS for the analysis of flonicamid was established. The samples were extracted by acetonitrile–methanol mixture and were purified using PSA. At fortification levels of 0.01, 0.1 and 0.5 mg/kg in cucumber, apple and soil, recoveries ranged from 71.5 to 106.0% with relative standard deviation (RSD) of 2.6–9.9%. The limit of quantification (LOQ) was 0.003 mg/kg for cucumber, apple and soil. This study also investigates the dissipation of flonicamid in cucumber, apple and soil. The dissipation half-lives of flonicamid in cucumber, apple and soil were 3.0–4.9 days, 5.1–6.1 days and 10.3–14.2 days, respectively. The final residues of flonicamid ranged from 0.029 to 0.295 mg/kg in cucumbers, <0.01–0.174 mg/kg in apples and <0.01–0.172 mg/kg in soil, respectively. The observed low residual levels of flonicamid suggest that the cucumber and apple are safe when applied at the recommended dosage.     

Monitoring residue levels and dietary risk assessment of pymetrozine for Chinese consumption of cauliflower

The present study investigates the occurrence of pymetrozine residues in cauliflower samples obtained from six cauliflower‐producing areas of China during fixed time periods in 2017 and estimates the dietary risk of pymetrozine in cauliflower. A liquid chromatography with tandem mass spectrometry method was developed and validated to detect pymetrozine in cauliflower. The samples were extracted using 20 mL of acetonitrile and purified with dispersive solid‐phase extraction using C₁₈ as sorbent. The limit of quantification of pymetrozine was 0.008 mg/kg in cauliflower. The recoveries of the analyte were 82.04–95.18% with RSD <8.45%. The calibration curves for pymetrozine showed good linearities in the concentration range 0.004–2.0 mg/L with determination coefficients (R²) >0.999. Pymetrozine dissipated rapidly in cauliflower with a half‐life of <4 days. The terminal residues of pymetrozine were <0.008–0.0881 mg/kg in cauliflower at 7, 10 and 14 days after spraying from six sites. The routine washing process removed about half amount of the pymetrozine in cauliflower; the reduction ratios were 51.0–52.8%. The dietary risk assessment indicated that pymetrozine did not exhibit obvious dietary health risks in cauliflower when good agricultural practices were implemented.     

Standardisation of cooking and conditioning methods for preparation of quick cooking germinated brown rice

Quick cooking germinated brown rice (QCGBR) is a novel convenient food product with valuable health benefits. Different cooking and conditioning methods were studied for standardisation of its preparation process. Freshly harvested paddy of Prativa variety was milled in rubber roll sheller to get brown rice which was soaked in demineralised water at 30 ​± ​2 ​°C for 12 ​h followed by 24 ​h of germination in an incubator maintained at 27 ​± ​1 ​°C temperature and 85–90% relative humidity to obtain germinated brown rice. The germinated brown rice was immediately cooked using three different cooking methods such as atmospheric cooking at normal ambient pressure, pressure cooking with water in a domestic pressure cooker at 1 ​bar gauge pressure and pressure steaming (without water) with steam at 1 ​bar gauge pressure to predetermined cooking time. The cooked samples after washing were then conditioned by keeping them at 4 ​°C for 24 ​h (refrigerated storage) or −10 ​°C for 24 ​h (frozen storage) in a house hold refrigerator. The stored samples were taken out after 24 ​h and tempered for 1 ​h followed by drying in a tray dryer at 90 ​°C to obtain the quick cooking germinated brown rice. The samples obtained from different cooking and conditioning methods were analysed for cooking quality, physico-chemical parameters, damaged grain percentage, GABA content and sensory attributes to standardise the cooking and conditioning methods. Cooking time, water uptake ratio, solid loss and volume expansion ratio of quick cooking germinated brown rice varied significantly with cooking and conditioning methods of its preparation (p ​< ​0.05). Though frozen conditioning resulted in lowest cooking time, it was not accepted by the sensory panel due to high damaged grain percentage, distorted shape and softness after cooking. The QCGBR obtained by pressure cooking method followed by refrigerated conditioning resulted in highest sensory score.     

高效液相色谱法同时测定稻田中苄嘧磺隆和苯噻酰草胺残留

建立了同时测定稻田(稻田土壤、水和植株)中苄嘧磺隆和苯噻酰草胺残留量的高效液相色谱(HPLC)分析方法。稻田水样品用二氯甲烷直接萃取;稻田土壤样品用碱性乙腈-二氯甲烷(1:1, v/v)混合液直接提取;水稻植株样品用碱性二氯甲烷提取后,二氯甲烷提取液经弗罗里硅土柱净化。上述样品溶液采用C18不锈钢色谱柱(150 mm×4.6 mm, 5 μm)分离,流动相为水-甲醇(30:70, v/v),流速为0.5 mL/min,柱温为30 ℃,紫外检测波长为238 nm,外标法定量。苄嘧磺隆和苯噻酰草胺在0.05～5.00 mg/L范围内的线性关系均很好(r＞0.9999)。在稻田水、土壤和水稻植株中添加3个水平(0.05, 0.10, 1.00 mg/kg)的苄嘧磺隆和苯噻酰草胺,两者的回收率均在85.39%～113.33%之间,相对标准偏差为0.91%～10.24%。这表明该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。     

酸性水稻土有效态砷与糙米砷含量相关性的研究

为了更好地探究酸性水稻土中有效态砷和糙米砷含量的相关性,采用土液比1:10、振荡时间240 min和振荡速度200 r·min-1为中间条件,比较4种浸提剂0.01 mol·L-1 CaCl2-DTPA,0.5 mol·L-1 NaHCO3,0.05 mol·L-1 NH4H2PO4和0.43 mol·L-1 HNO3提取酸性水稻土中有效砷的提取效果。结果表明,4种浸提剂提取的土壤有效态砷与其糙米砷含量之间均存在显著相关,0.43 mol·L-1 HNO3提取的土壤有效态砷与糙米砷含量的相关性最高为0.828,土壤有效态砷平均提取率最高为8.63。选择0.43 mol·L-1 HNO3为提取酸性水稻土有效态砷的最优浸提剂,进一步优化浸提剂的提取条件,确定土液比1:10、振荡时间120 min和振荡速度200 r·min-1为酸性水稻土有效态砷最佳提取条件,土壤有效态砷与糙米砷含量的相关性最高为0.831。0.43 mol·L-1 HNO3提取酸性水稻土中有效砷的方法操作简便、试剂用量少,提取的土壤有效砷和糙米砷的相关性好,确定为酸性水稻土有效态砷的提取方法,为科学评价酸性水稻土壤有效态砷与糙米砷的生物有效性以及酸性水稻土壤砷环境风险评价提供参考依据。     

Dissipation,residues and risk assessment of spirotetramat and its four metabolites in citrus and soil under field conditions by LC‐MS/MS

A modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for the simultaneous determination of spirotetramat and its four metabolite residues in citrus, peel, pulp and soil was developed and validated by liquid chromatography with tandem mass spectrometry (LC‐MS/MS). The samples were extracted with acetonitrile (1%, glacial acetic acid, v/v) and purified using primary secondary amine and octadecylsilane. The limit of detection was 0.01–0.13 mg/kg, whereas that of quantification was 0.02–0.40 mg/kg for spirotetramat and its metabolites. The average recoveries of spirotetramat, spirotetramat‐enol, spirotetramat‐mono‐hydroxy, spirotetramat‐enol‐glucoside and spirotetramat‐ketohydroxy in all matrices were 73.33–107.91%, 75.93–114.85%, 76.44–100.78%, 71.46–103.19% and 73.08–105.27%, respectively, with relative standard deviations < 12.32%. The dissipation dynamics of spirotetramat in citrus and soil followed first‐order kinetics, with half‐lives of 2.3–8.5 days in the three sampling locations. The terminal residues of spirotetramat in four matrices at the three locations were measured below the 1.0 mg/kg maximum residue limit set by China, and residues were found to be concentrated on the peel. The risk assessment of citrus was evaluated using risk quotients. The risk quotient values were found to be significantly <1, suggesting that the risk to human health was negligible when using the recommended doses of spirotetramat in citrus. These results could provide guidance for the safe and proper application of spirotetramat in citrus in China.     

Analytical methods for pesticide residues in rice

Rice consumption has increased worldwide over recent decades, as it has become one of the most common foods. Although the analysis of environmental samples coming from rice areas has been well documented, there is less information regarding the analysis of pesticide residues in rice-grain samples.Rice (paddy, brown and white) can be considered a complex matrix, leading to difficulties in the application of the different multiresidue methods described in the literature. This review addresses and compares the principal extraction and clean-up methodologies [e.g., liquid-liquid extraction, solid-phase extraction, pressurized-liquid extraction, QuEChERS (quick, easy, cheap, effective, rugged and safe), gel-permeation chromatography and supercritical-fluid extraction - with QuEChERS-based methods being the most frequently employed].Traditionally, the determination of pesticide residues in rice has been based on gas chromatography with mass spectrometry (MS). But the application of new classes of pesticides has driven laboratories to increase the use of liquid chromatography with tandem MS. The limits of detection and quantification are in the ranges 0.09-90 μg/kg and 1-297 μg/kg, respectively, for the methodologies reported. These values agree with the current internationally-accepted maximum residue limits (MRLs).Based on the European Union (EU) database, more than 3000 analyses of pesticide residues in rice have been performed by official EU laboratories over the past decade. Of these, 6% reported pesticide residues above the MRLs.Physico-chemical properties can explain the occurrence of pesticides in rice commodities: lipophilic pesticides are frequently found in brown rice, whereas fungicides are mainly found in milled rice. Carbendazim, malathion, iprodione, tebuconazole, quinclorac and tricyclazole are the pesticides most frequently found in white rice, while buprofezin, hexaconazole, chlorpyrifos and edifenphos are most commonly found in paddy rice.Pesticide-residue concentrations can be affected during rice processing - with concentrations generally lower in the final products. However, few studies focusing on primary processing have addressed the setting of precise values applicable for the processing factors.     

QuEChERS-高效液相色谱法测定稻田土壤、糙米和秸秆中的灭草松残留

建立了一种稻田土壤、糙米和秸秆中灭草松残留量的QuEChERS-HPLC检测方法。以乙腈为提取溶剂,N-丙基-乙二胺(PSA)为吸附剂,实现样品快速制备;在C18色谱柱上,以甲醇-0.2‰H3PO4(55/45,V/V)为流动相,紫外检测器于215nm波长处检测,在0.1～5.0 mg/L范围内浓度与峰面积呈良好的线性关系,相关系数为0.9991。在添加浓度为0.05～1.0 mg/kg范围内的平均回收率为88.6%～96.8%,相对标准偏差为1.1%～2.7%,检出限为5.5×10-11g。方法能够满足水稻田土壤、糙米和秸秆样品中灭草松的残留检测。     

Determination of iodine-129 and iodine-127 in environmental samples collected in Japan

Analytical method for the determination of¹²⁹I and¹²⁷I in environmental samples has been developed by using radiochemical neutron activation analysis. The¹²⁹I levels in the samples such as soil (0.9–41 mBq/kg), precipitation (0.002–0.11 mBq/kg), pine needles (1.2–32 mBq/kg) and seaweed (<0.1–17 mBq/kg) collected near the nuclear facilities in Tokaimura were higher than those from the other areas in Japan. The highest¹²⁹I concentration was found in surface soil (0–5 cm), and the highest¹²⁹I/¹²⁷I ratios were found in pine needles and precipitation. The¹²⁹I/¹²⁷I ratio was higher in rice paddy soil than those in wheat field soil collected around Tokaimura, while the concentration of¹²⁹I somewhat higher in wheat field soil.     

Chromatographic determination,decline dynamic and risk assessment of sulfoxaflor in Asian pear and oriental melon

The dissipation pattern of sulfoxaflor in Asian pear cultivated in an open field conditions and in oriental melon grown under plastic house conditions was each studied in two different locations. Residues in field‐treated samples were determined using liquid chromatography coupled with an ultraviolet detector and confirmed by liquid chromatography–tandem mass spectrometry. A calibration curve for sulfoxaflor was linear over the concentration range 0.1–5.0 mg/L, with a coefficient of determination of 0.9999. The limits of detection and quantification (LOQ) were 0.007 and 0.02 mg/kg, respectively. Recoveries at three fortification levels (LOQ, 10 × LOQ and maximum residue limit) ranged from 70.5 to 86.2%, with a relative standard deviation ≤5.8%. The dissipation half‐lives were 10.8 and 7.9 days in pear and 5.4 and 5.9 days in oriental melon, at sites 1 and 2, respectively. Based on a pre‐harvest residue limit curve, it was predicted that, if the residues at 10 days before harvest in Asian pear are <0.54/0.61 mg/kg and those in oriental melon are <1.43/1.26 mg/kg, then the residue level will be below the maximum residue limit at harvest. Risk assessment at zero days showed a percentage acceptable daily intake of 10.80% in Asian pear and 1.77 and 1.55% in oriental melon, for sites 1 and 2, respectively. These values indicate that the fruits are safe for consumption.     

Effects of active silicon uptake by rice on 29Si fractionation in various plant parts

Rice (Oryza sativa L.) accumulates large amounts of silicon which improves its growth and health due to enhanced resistance to biotic and abiotic stresses. Silicon uptake and loading to xylem in rice are predominantly active processes performed by transporters encoded by the recently identified genes Lsi1 (Si influx transporter gene) and Lsi2 (Si efflux transporter gene). Silicon deposition in rice during translocation to upper plant tissues is known to discriminate against the heavier isotopes ²⁹Si and ³⁰Si, resulting in isotope fractionation within the plant. We analyzed straw and husk samples of rice mutants defective in Lsi1, Lsi2 or both for silicon content and δ²⁹Si using isotope ratio mass spectrometry (IRMS) and compared these results with those for the corresponding wild‐type varieties (WT). The silicon content was higher in husk than in straw. All the mutant rice lines showed clearly lower silicon content than the WT lines (4–23% Si of WT). The δ²⁹Si was lower in straw and husk for the uptake defective mutant (lsi1) than for WT, albeit δ²⁹Si was 0.3‰ higher in husk than in straw in both lines. The effect of defective efflux (lsi2) differed for straw and husk with higher δ²⁹Si in straw, but lower δ²⁹Si in husk while WT showed similar δ²⁹Si in both fractions. These initial results show the potential of Si isotopes to enlighten the influence of active uptake on translocation and deposition processes in the plant. Copyright © 2009 John Wiley & Sons, Ltd.     

Simultaneous determination of trifloxystrobin and trifloxystrobin acid residue in rice and soil by a modified quick,easy, cheap,effective, rugged,and safe method using ultra high performance liquid chromatography with tandem mass spectrometry

A sensitive analytical method for the simultaneous determination of trifloxystrobin and its metabolite trifloxystrobin acid in rice including straw, bran, brown rice and soil was developed by using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The fungicide trifloxystrobin and its metabolite trifloxystrobin acid were extracted using acetonitrile with 1% formic acid v/v and subsequently cleaned up by primary secondary amine, octadecylsilane or graphitized carbon black prior to ultra high performance liquid chromatography coupled with tandem mass spectrometry. The determination of two target compounds was achieved in less than 3 min using an electrospray ionization source in positive mode. The limits of detection were below 0.22 μg/kg and the limits of quantification did not exceed 0.74 μg/kg in all matrices, which were much lower than the maximum residue levels established by the Codex Alimentarius Commission. The overall average recoveries in four matrix at three levels (0.1, 1.0 and 5.0 mg/kg) ranged from 74.2 to 107.4% with a relative standard deviations of less than 7.8% (n = 5) for both analytes. The method was demonstrated to be convenient and reliable for the routine monitoring of trifloxystrobin and its metabolite. The developed method was validated and applied for the analysis of degradation study samples.