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1.
Dissipation and residue levels of bifenthrin and chlorfenapyr in eggplant and soil under field conditions were investigated using gas chromatography coupled with an electron capture detector (GC-ECD). The mean recoveries of bifenthrin and chlorfenapyr were 85.2–104.9%, with relative standard deviations (RSDs) of 0.5–9.1%. The limit of quantification (LOQ) was 0.01 mg kg?1. Bifenthrin exhibited half-lives of 3.3 to 4.1 days in eggplant and 17.8 to 25.7 days in soil; the half-lives of chlorfenapyr were 3.5 to 3.8 days in eggplant and 21.7 to 27.7 days in soil. During harvest, the terminal residues of bifenthrin and chlorfenapyr were below 0.031 and 0.083 mg kg?1, respectively. Risk assessment for different groups of people in China was evaluated. The risk quotients (RQs) of bifenthrin and chlorfenapyr were ranged from 0.0068 to 0.0148 and from 0.0033 to 0.0072, respectively. These results may provide guidance on reasonable use of pesticides and serve as a basis for establishing maximum residue limits (MRLs) in China.  相似文献   

2.
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.  相似文献   

3.
An ultra high‐performance liquid chromatography with tandem triple quadrupole mass spectrometry residue method was developed and validated for the quantification and identification of dinotefuran and its main metabolites 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) urea and 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) guanidine in fruit (watermelon), vegetable (cucumber), cereal (rice), animal‐derived foods (milk, egg, and pork), soil, and water. The samples were extracted with acetonitrile containing 15% v/v acetic acid and purified with dispersive solid‐phase extraction with octadecylsilane, primary secondary amine, graphitized carbon black, or zirconia‐coated silica prior to analysis. The method had an excellent linearity (R2 ≥ 0.9942, 1–500 μg/L) and satisfactory recoveries (73–102%) at five spiked levels (0.001, 0.01, 0.05, 0.5, and 2 mg/kg) with intra‐ or interday precision in the range of 0.8–9.5% and 3.0–12.8% for the three compounds in the eight matrices. The limits of quantification were 10 μg/kg for 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) guanidine and 1 μg/kg for 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) urea and dinotefuran. The applicability of the developed method was demonstrated by determining the occurrence of dinotefuran, 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) guanidine, and 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) urea in various samples from plants, animal‐derived foods, and the environment. From 80 samples, 70 contained dinotefuran (0.8–11.7 μg/kg), among which six also contained 1‐methyl‐3‐(tetrahydro‐3‐furylmethyl) urea (water and rice, 0.5–0.9 μg/kg).  相似文献   

4.
ABSTRACT

A simple, rapid and selective method based on liquid chromatography tandem mass spectrometry and QuEChERS was established for simultaneous determination of dimethomorph and benthiavalicarb-isopropyl residues in grape. The mean intra-day recoveries of dimethomorph and benthiavalicarb-isopropyl in grape were in the range of 91.5–103.5% at four-spiked levels. The inter-day recoveries of dimethomorph and benthiavalicarb-isopropyl in grape were 98.9% and 98.6% at spiked level of 0.5 mg kg?1, respectively. The relative standard deviation (RSD) was lower than 8.4%, and the limit of quantitation (LOQ) was 0.01 mg kg?1 for both fungicides. The residual behaviour of both fungicides in the grape field at two different locations was investigated using the developed and validated method. The half-lives of dimethomorph in grapes were 5.9 to 8.8 d, and that of benthiavalicarb-isopropyl were 7.9 to 11.6 d. The terminal residues of dimethomorph and benthiavalicarb-isopropyl were lower than 1.3 and 0.79 mg kg?1, respectively. The results of dietary risk assessment showed that the risk of dimethomorph and benthiavalicarb-isopropyl was negligible to Chinese residents.  相似文献   

5.
Pesticide residue in food commodities is a serious concern in relation to consumer safety and also the most significant barrier in the trade of food commodities. The dissipation pattern of four insecticides, namely novaluron, λ-cyhalothrin, imidacloprid, and fenazaquin, was evaluated on tomato fruits and cropped soil. The residues were extracted using the QuEChERS analytical method and quantized using a gas chromatograph with electron capture detector, gas chromatograph mass spectrometer, and high-performance liquid chromatography with photo diode array detector. The analytical method was validated using parameters like recovery, linearity, accuracy, matrix effect, and specificity, with limit of detection and limit of quantitation established to be 0.01 and 0.05 mg/kg, respectively, for all the pesticides. The average initial deposits (samples collected after 2 h of application) at the recommended dose of novaluron, λ-cyhalothrin, imidacloprid, and fenazaquin were 0.593, 0.293, 0.227, and 0.431 mg/kg on tomato fruits, respectively, and were below the limit of quantification in soil. The pre-harvest interval of 17, 8, 1, and 13 days was suggested for novaluron, λ-cyhalothrin, imidacloprid, and fenazaquin on tomato, respectively. Risk assessment studies revealed that all pesticides under study are safe and do not pose any threat to humans as theoretical maximum dietary intake is less than the maximum permissible intake and acceptable daily intake.  相似文献   

6.
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.  相似文献   

7.
Residue analysis of dimethomorph in Swiss chard cultivated at two different locations under greenhouse conditions was conducted using high‐performance liquid chromatography–ultraviolet detection and confirmed by tandem mass spectrometry. The randomly collected samples (over 14 days) were extracted with acetonitrile and purified using a Florisil solid‐phase extraction cartridge. Linearity over a concentration range of 0.05–50.0 mg/L had an excellent coefficient of determination of 0.9996. Recovery rate ranged from 82.98 to 95.43% with relative standard deviations ≤5.12% and limits of detection and quantification of 0.003 and 0.01 mg/kg, respectively. The initial deposits [day 0 (2 h post‐application)] were considerably lower (7.57 and 8.55 mg/kg for sites 1 and 2, respectively) than the maximum residue limit (30 mg/kg) set by the Korean Ministry of Food and Drug Safety. The dissipation half‐life was approximately the same, being 5.0 and 5.1 days for sites 1 and 2, respectively. Risk assessment estimated as acceptable daily intake revealed a value of 0.084 or 0.094% (day 0) and 0.014% (10 days post‐application), for sites 1 and 2, respectively. The values indicated that dimethomorph can be safely used on Swiss chard, with no hazardous effects expected for Korean consumers.  相似文献   

8.
为研究黔产市售鱼腥草中铅、镉、铬、砷4种重金属的含量水平及其膳食健康风险水平。以贵州贵阳(GY)、遵义(ZY)、铜仁(TR)、安顺(AS)、毕节(BJ)、六盘水(LPS)、黔东南(QDN)、黔西南(QXN)、黔南(QN)等9个市(州)市售鱼腥草为研究对象,利用微波消解处理样品,采用电感耦合等离子体质谱(ICP-MS)法同时测定样品中的4种重金属含量,利用单因子污染指数法、内梅罗综合污染指数法对重金属的污染程度进行评价,利用目标危害系数法进行膳食风险评估。结果显示,鱼腥草中Pb含量为0.084~0.12 mg/kg, Cd含量为0.041~0.068 mg/kg, Cr含量为0.076~0.43 mg/kg, As含量为0.074~0.14 mg/kg。TR、QDN、ZY市售鱼腥草Pb的单项污染指数均大于1,9个市(州)市售鱼腥草Cd、Cr、As的单项污染指数均小于1。不同市(州)市售鱼腥草的内梅罗综合污染指数大小次序为1>TR>QDN>ZY>AS>GY>BJ>QXN>0.7≥QN>LPS。单一重金属的膳食健康风险指数(THQ)总体上...  相似文献   

9.
In this study, a sensitive and reliable analytical method, based on a modified Quick, Easy, Cheap, Effective, Rugged and Safe procedure, was established for determination of tebuconazole in jujube. After extraction with acetonitrile, the samples were cleaned up by dispersive solid‐phase extraction with primary secondary amine, and determined by high‐performance liquid chromatography tandem mass spectrometry. At fortification levels of 0.01, 0.1 and 2.0 mg kg−1, the average recoveries of tebuconazole in jujube were in the range 97.6–101.9%, with relative standard deviations of 1.5–3.5%. The dissipation and residual levels of tebuconazole in jujube under field conditions were investigated. Tebuconazole dissipated relatively slowly in jujube, with a half‐life of 33.0 days. The terminal residue experiments of tebuconazole in jujube were conducted in four locations in China and the risk was evaluated using risk quotients (RQ ). RQ values were found to be significantly lower than RQ = 1, indicating that the risk to human health of using the recommended doses of tebuconazole in jujube was not significant. This study could provide guidance for the safe and reasonable use of tebuconazole in jujube and serve as a reference for the establishment of limit of maximum residue in China.  相似文献   

10.
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.  相似文献   

11.
A liquid chromatography with tandem mass spectrometry method was developed and validated to simultaneously determine chlorpyrifos, imidacloprid, and imidacloprid metabolites in soil, wheat grain, and wheat straw matrices. Satisfactory linearity (R2 ≥ 0.9965) of the method was obtained for all analytes. The ranges of limits of detection and limits of quantification for seven analytes in three matrices were 0.17–66.7 and 0.5–200 μg/kg, respectively. Average recoveries were 72.85–81.25% for chlorpyrifos, 78.54–84.70% for imidacloprid, 73.83–81.03% for imidacloprid olefin, 71.47–80.61% for 5‐hydroxy imidacloprid, 71.79–81.32% for imidacloprid urea, 70.42–82.20% for imidacloprid nitroguanidine, and 70.91–82.46% for imidacloprid 6‐chloronicotinic acid in soil, wheat grain, and wheat straw. The intra‐ and interday relative standard deviations were less than 8%. The established method was successfully applied for the residual analysis of chlorpyrifos, imidacloprid, and imidacloprid metabolites in actual soil, wheat grain, and wheat straw samples. The results indicated that the established method could be used to detect trace amounts of chlorpyrifos, imidacloprid, and imidacloprid metabolites in wheat and that the method might be able to provide some data on the detection of these seven compounds in other crops.  相似文献   

12.
云南阳宗海砷污染水平、变化趋势及风险评估   总被引:7,自引:0,他引:7       下载免费PDF全文
云南阳宗海砷污染事件引起社会广泛关注.为了解事件发生后阳宗海砷污染水平及变化趋势,分别于2008年12月、2009年2月、5月及9月四次采样,研究了阳宗海湖水、底泥、周边井水、土壤、农作物及水生生物中的砷含量及其变化趋势.研究结果显示:湖水平均砷浓度分别为176.9、147.3、159.3和161.1μg/L(算术平均),底泥平均浓度分别为32.87、62.41、62.99和46.96μg/g(算术平均).阳宗海湖水砷浓度经历了先升后降再到平稳的变化过程,底泥砷含量迅速升高后缓慢下降,湖水和底泥间砷交换还在进行.阳宗海附近土壤中砷最高浓度为23.33μg/g,未超过国家土壤环境质量三级标准.大米、玉米、花椰菜、小油菜等农作物可食用部分中砷的最高值为0.35μg/g,均未超过国家无公害食品标准.水生植物中砷水平大多在100~200μg/g之间,最高为苦草,砷含量超过300μg/g,说明该植物对砷有一定的富集能力.虾、鱼类等可食用水生动物砷浓度范围为1.52~11.4μg/g.  相似文献   

13.
Summary Propafenone (PPF) is a new antiarrhythmic agent with structural features in common with the class of beta-blocking drugs (phenoxypropanolamines). Because of its high lipophilicity, the drug is strongly retained in reverse phase (RP) columns and simultaneous determination with the main polar metabolites 5-OH-PPF, N-depropyl-PPF and 5-OH-4-methoxy-PPF requires long run times (up to 50 min.) Oxidative metabolism in vivo often produces derivatives whose higher polarity results from the addition of a polar group and/or the subtraction of an apolar one. These metabolites show similar chromatographic behaviour in RP mode and the trade-off between their separation and the sensitivity of the parent compound must be investigated. In an effort to shorten the run time we examined the retention of these early eluting substances as a function of different amine additives, pH and organic content in mobile phase using C8 and C-18 columns from different sources, previously characterized for their free silanophilic and hydrophobic activities. Under optimal conditions the run time was reduced to 14 minutes and an application of the optimized method to the determination in plasma samples of the drug and its main metabolites after chronic therapy with PPF is presented. To investigate possible coelution of other yet undiscovered metabolites which could accumulate in some patients under chronic treatment, the analysis was carried out using an electrochemical detection in parallel with the UV. Agreement was found between the two detection procedures and suggest no interference.  相似文献   

14.
Summary Direct chiral-phase HPLC methods have been developed for the determination of flurbiprofen and its major metabolites, namely 4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen, in biological fluids using a derivatized amylose chiral stationary phase (CSP; Chiral-pak AD). Quantification of all three analytes, both free and conjugated, in urine was carried out following liquid-liquid extraction using tandem ultraviolet (UV) and fluorescence detection. Determination of flurbiprofen and the 4′-hydroxy-metabolite in plasma utilized the same CSP but required modification in the mobile phase composition and sole use of fluorescence detection. The urine assay was linear (r>0.998) between 0.05–10 μg mL−1, 0.1–20 μg mL−1 and 0.01–2 μg mL−1 for the enantiomers of flurbiprofen, 4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen respectively. The plasma assay was linear (r>0.997) between 0.1–6 μg mL−1 and 0.01–0.6 μg mL−1 for the enantiomers of flurbiprofen and 4′-hydroxyflurbiprofen respectively. Both assays, typically yielded within- and between-day imprecision and accuracy values less than 10% for the enantiomers of the different analytes. Initial volunteer studies suggest that the disposition of flurbiprofen displays modest enantioselectivity in humans.  相似文献   

15.
This study presents the method development, validation, and simultaneous determination of dimethoate and its metabolite omethoate in curry leaf. Samples were extracted following modified quick, easy, cheap, effective, rugged, and safe extraction protocol and analyzed using liquid chromatography-tandem mass spectrometry. The limit of quantification in the matrix was 0.005 μg g−1 for dimethoate and omethoate. Extraction using acetonitrile recorded the average recoveries in the range of 82.25 to 112.97% for dimethoate and 85.57 to 107.22% for omethoate at 0.005, 0.025 and 0.050 μg g−1 fortification levels and relative standard deviation less than 5%. Similarly, the relative standard deviation values for intraday (Repeatability) and interday (Reproducibility) tests were less than 15%. Dissipation kinetics of dimethoate 30% emulsifiable concentrate at 200 and 400 g a.i h−1 recorded initial deposits of 5.20 and 10.05 μg g−1 and 0.33 and 0.48 μg g−1 for dimethoate and omethoate, respectively, and half-life of 3.07 and 3.34 days. The estimated hazard index value found more than one at a day after dimethoate application. It is not safe for consumer health to use curry leaves in the initial days after application.  相似文献   

16.
A simple and efficient multiresidue method using dispersive solid phase extraction and liquid chromatography coupled with tandem mass spectrometry was developed for the targeted analysis of indaziflam and its five metabolites (indaziflam‐diaminotriazine, indaziflam‐carboxylic acid, indaziflam‐triazine indanone, indaziflam‐hydroxyethyl, and indaziflam‐olefin) in pitaya samples (including roots, plants, flowers, peels, pulp, and whole fruit). The analytes were extracted with acetonitrile, and the extracts were purified using multiwalled carbon nanotubes. The method was validated using pitaya samples spiked at 0.5, 5, and 50 µg/kg, and the average recoveries varied from 61.1 to 103.7% with relative standard deviations lower than 12.7% (= 5). This method exhibited sufficient linearity within the concentration range of 0.1–100 µg/L. The limits of detection and quantification were in the ranges of 0.001–0.1 and 0.003–0.3 µg/kg, respectively. The method was successfully applied to analyze pitaya samples in Nanning, and no indaziflam or its metabolites were detected in the samples analyzed.  相似文献   

17.
ABSTRACT

This study was conducted to investigate the residues of pyrethroid and organophosphorus pesticide in flour and breads which were collected from local markets in Kermanshah province, Iran. Four different types of breads and two types of flour samples with high distribution were taken from market and their residues of pesticides were measured. A simple dispersive liquid–liquid microextraction (DLLME) method with solidification of floating organic drop was developed for the measurement. The health risk of these pesticides on adults and children health was assessed by target hazard quotient (THQ) using Monte Carlo simulation (MCS) method. About, 15% and 11.1% of total samples contained detectable levels of deltamethrin and malathion, respectively. None of the tested samples showed any permethrin residue. The results from all samples showed that none of the pesticides exceeded the maximum residue limits (MRLs). About 85% of pesticide residue detections were observed in tropical and mild weather area which is due to high consumption rate of insecticides in these areas. The percentile 95% of THQ is due to bread ingestion content of deltamethrin which was 0.033 and 0.070 for the adults and children, respectively, while this value for malathion was found to be, 0.015 and 0.030, respectively. In the adults and children for both deltamethrin and malathion, the percentile 95% of THQ value were lower than 1 (acceptable level). The non-carcinogenic health risk assessment indicated that bread consumers in Kermanshah province are not at a considerable risk because of deltamethrin and malathion.  相似文献   

18.
Aromatic solvents are involved in manifold areas of industry and craft. Inhaled solvent vapors are a known health hazard to workers. For medical prevention and toxicological assay specific laboratory methods for urinary metabolites are necessary. An economical capillary gas chromatographic procedure is described which is suitable for routine analysis of major metabolites, sensitive for the determination of minor metabolites, and effective for the separation of chiral metabolic intermediates.  相似文献   

19.
Summary An HPLC method with electrochemical detection has been developed for the determination of clozapine and its main metabolites, desmethylclozapine and clozapine N-oxide, in human plasma. An accurate pretreatment of the biological samples was implemented by means of solid phase extraction (SPE) on HLB cartridges. This improved pretreatment, together with a new mobile phase, allows for the accurate determination of clozapine N-oxide, which could not be quantitated by a previous method. The method uses only 100 μL of plasma for one complete analysis and shows good recovery values for all three analytes. The eluates from the SPE procedure were chromatographed in a reversed phase C18 column using a mobile phase composed of phosphate buffer, acetonitrile and methanol. Clozapine, desmethylclozapine and clozapine N-oxide were eluted in less than 10 minutes, without any interference from the biological matrix. Linearity was observed over the 2.50–150 ng mL−1 (clozapine and desmethylclozapine) or 1.25–75 ng mL−1 clozapine N-oxide) range for the three analytes, with satisfactory repeatability values. The limit of detection was 0.3 ng mL−1 for clozapine and desmethylclozapine, samples of patients treated with Leponex gave good results. No interference from other common central nervous system drugs was found. This method seems to be a useful tool for pharmacokinetic studies and for clinical monitoring, because of its need for small plasma samples and its high sensitivity and selectivity.  相似文献   

20.
As chlorpyrifos is used globally to control pests in sugarcane fields, analysis of its residues on food crops is essential to assess product safety for humans. In this study, chlorpyrifos content in sugarcane plants, soil and juice was determined using a gas chromatography with an electron capture detector. The limit of quantification was 0.01 mg/kg for plant and soil, and 0.01 mg/L for juice. The degradation and residual risk in sugarcane fields after applying chlorpyrifos to two sample sites (Changsha and Danzhou, China) were assessed. Chlorpyrifos concentrations in plants and soil decreased rapidly over time, reaching a degradation rate ranging from 98.82 to 99.25% on day 35. The half‐life of chlorpyrifos in both plants and soil was only 5.97–6.12 days. Regardless of application dosage (standard or high) at a pre‐harvest interval of 60 days, chlorpyrifos was undetectable in the harvested sugarcane. Risk assessment indicated that chlorpyrifos residue in sugarcane did not pose a health risk to humans.  相似文献   

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