Elemental Analysis of Edible Mountain Nettle (Obetia tenax) and the Influence of Soil on Its Chemical Composition

In developing countries, the dietary intake of essential elements is largely dependent on the consumption of edible fruits and leafy vegetables. The distribution of elements in the indigenous edible plant, Obetia tenax (mountain nettle), was investigated as a function of soil quality from eight sites in KwaZulu-Natal, South Africa. The results show concentrations of elements in the leaves to be in decreasing order of Ca?>?Mg?>?Fe?>?Mn?>?Zn?>?Cr?>?Cu?>?Ni?>?Pb?>?Co?>?As?>?Cd?>?Se, and in the stems and roots to be in decreasing order of Ca?>?Mg?>?Fe?>?Mn?>?Zn?>?Cu?>?Ni?>?As?>?Pb?>?Co?>?Cd?>?Cr?>?Se. The quality and pollution status of soil was evaluated by geoaccumulation indices and enrichment factors, which indicated moderate cadmium contamination at the Msinga location that was confirmed by the pollution index and ecological risk levels of single-factor pollution. An assessment of overall contamination of soil using Nemerow pollution index showed moderate pollution by cadmium, while the potential toxicity index indicated low-grade risk for all elements at all sites. Principal component and cluster analysis revealed two groups of elements with similarities, As, Cd, Co, Cr, Cu, Mn, Ni, and Fe, suggesting a lithogenic source and an anthropogenic source for Pb and Zn. Correlation analysis showed significantly positive correlations between As, Co, Cr, Cu, Fe, and Ni/Cd in the soil, confirming the elements’ common origin.     

Determination of fipronil and its major metabolites in vegetables,fruit and soil using QuEChERS and gas chromatography-mass spectrometry

A rapid, simple and selective gas chromatography with mass spectrometric detection (GC-MS) method was developed and validated for simultaneously determining fipronil and its three major metabolites in vegetables, fruit and soil. The fipronil residues were extracted using QuEChERS technique with ethyl acetate and then were purified by dispersive solid phase extraction (d-SPE) cleanup for cabbage, cauliflower, okra, tomato, grapes and soil. The linearity of the analytical response across the studied range of concentrations (0.01–0.5?µg?mL^?1) was excellent, obtaining correlation coefficients higher than 0.999. The average recoveries of the pesticide from all matrixes ranged from 86 to 112%, for fortification levels of 0.01, 0.05 and 0.1?µg?g^?1. The precision values associated with the analytical method, expressed as RSD values, were less than 10.15% for the pesticide in all matrixes. This method can be used to evaluate environmental residues and the safety of agricultural products.     

Autotoxicity and allelopathy of 3,4-dihydroxyacetophenone isolated from Picea schrenkiana needles

Bioassay-guided fractionation of the diethyl ether fraction of a water extract of Picea schrenkiana needles led to the isolation of the phenolic compound 3,4-dihydroxy- acetophenone (DHAP). The allelopathic effects of DHAP were evaluated under laboratory conditions on P. schrenkiana, rice (Oryza sativa L.), wheat (Triticum aestivum L.), radish (Raphanus sativus L.), lettuce (Latuca sativa L.), cucumber (Cucumis sativus L.) and mung bean (Phaseolus radiatus L.). DHAP significantly inhibited seed germination and seedling growth of P. schrenkiana at concentrations of 2.5 mM and 0.5 mM (p < 0.05). Soil analysis revealed that P. schrenkiana forest soils contained exceptionally high DHAP concentrations (mean = 0.51 ± 0.03 mg/g dry soil), suf?cient to inhibit natural P. schrenkiana recruitment. DHAP also exhibited strong allelopathic potential. It significantly inhibited wheat and lettuce seed germination at concentrations of 1 mM and 0.5 mM (p < 0.05). The active compound also completely inhibited root growth of the six test species at high concentrations. Our results suggest a dual role of DHAP, both as an allelochemical and as an autotoxicant. The potential for a single plant needle-leached compound to in?uence both inter- and intra-speci?c interactions emphasized the complex effects that plant secondary metabolites might have on plant population and community structure.     

Determination of Essential and Toxic Elements in Vegetables from South Korea

This study reports the determination of trace essential (Co, Cr, Cu, Se, and Zn) and toxic (Al, As, Cd, Hg, and Pb) elements in greenhouse tomatoes, peppers, and cucumbers from supermarkets of Seoul, Busan, Gangneung, Daegu, Daejeon, and Gwangju, South Korea using inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectroscopy, and direct mercury analysis. The methods were validated by linearity, limits of detection and quantification, precision, accuracy, and recovery measurements that provided satisfactory results in all cases. Among the essential trace elements, Zn was found to have the highest concentrations (0.84–2.5?mg/kg) followed by Cu (0.21–0.62?mg/kg) and Cr (0.01–0.06?mg/kg). The mean concentrations (mg/kg) of the toxic elements were in the order Al?>?Pb?>?As?>?Cd?>?Hg for tomatoes and cucumbers and Al?>?Pb?>?Cd?>?As?>?Hg for peppers; all were below the permissible limits set by World Health Organization for human consumption. The estimated dietary intake, target hazard quotients (THQs), and hazard indices of the samples were within safe levels. The combined THQ values for the toxic elements in the vegetables were from 0.002 to 0.012 with significant contribution from arsenic, aluminum, cadmium, and mercury. The results of this study show that trace and toxic elements in the analyzed vegetables do not impose any serious health harmful effects for the population upon consumption.     

Distribution and Assessment of Heavy Metals in Trifolium dubium (Little Hop Clover) and the Impact of Soil Quality

Trifolium dubium is an edible plant that is utilized in traditional medicine for its anti-inflammatory and wound-healing properties. In this study, T. dubium was assessed to determine the elemental uptake by the plant as a function of soil characteristics. Across 10 geographic locations in KwaZulu-Natal, South Africa, the concentration of elements in T. dubium were found to be (descending order) Ca?>?Mg?>?Fe?>?Zn?>?Mn?>?Se?>?Ni?>?Cr?>?Cu?>?Co?>?Pb?>?Cd?>?As. The site had an influence on elemental uptake by the plant; however, accumulation or exclusion of elements from soil was controlled to meet physiological requirements. Soil chemical characteristics showed T. dubium grew in slightly acidic soils (pH – 6.15 to 6.68). The findings of this study show T. dubium to contain adequate concentrations of essential elements with undetectable levels of toxic metals, making the herb safe for human consumption and for use in traditional medicine. The plant can also contribute to poor communities by ameliorating food insecurity.     

多壁碳纳米管固相萃取净化气相色谱法分析蔬菜中有机氯和拟除虫菊酯农药残留

建立了多壁碳纳米管为吸附剂的固相萃取(SPE)净化、气相色谱-电子捕获检测(GC-ECD)测定蔬菜中6种有机氯和7种拟除虫菊酯农药的方法。采用双柱(HP-50和HP-1色谱柱)双检测器进行定性和定量分析。蔬菜样品采用乙腈提取,多壁碳纳米管SPE柱净化,正己烷溶解上样,丙酮-正己烷(7:3, v/v)洗脱,13种农药中有11种农药的添加回收率高于70%。将该净化方法用于荷兰黄瓜、卷心菜、红圣女果、奶油生菜、紫甘蓝、韭菜、大葱和洋葱等样品的净化,与弗罗里硅土SPE柱相比较,净化效果更好,表明多壁碳纳米管具有较强的吸附去除色素的能力,可以避免色素对测定的干扰。     

Enantioselective separation and simultaneous determination of fenarimol and nuarimol in fruits, vegetables, and soil by liquid chromatography–tandem mass spectrometry

A method for simultaneous enantioselective determination of fenarimol and nuarimol in apple, grape, cucumber, tomato, and soil was developed using liquid chromatography–tandem mass spectrometry. The enantioseparation results of the two fungicides through three different cellulose-based chiral columns are discussed. The influence of column temperature on the resolution of the enantiomers of the two fungicides was examined. Complete enantioseparation of the two fungicides’ enantiomers was obtained on a cellulose tris(4-methylbenzoate) column (Lux Cellulose-3) at 25?°C using methanol and 0.1?% formic acid solution (80:20, v/v) as mobile phase. The linearity, matrix effect, recovery, and precision were evaluated. Good linearity was obtained over the concentration range of 1–500?μg?L^?1 for each enantiomer in the standard solution and sample matrix calibration solution. There was no significant matrix effect in apple, grape, cucumber, or tomato samples, but signal suppression was typically observed with the soil extracts. The mean recoveries, repeatability, and reproducibility were 76.5–103?%, 2.1–9.0?%, and 4.2–11.8?%, respectively. The limit of quantification for enantiomers of the two fungicides in fruits, vegetables and soil was 5?μg?kg^?1. Moreover, the absolute configuration of the enantiomers of fenarimol and nuarimol was determined from a combination of experimentally determined and predicted electronic circular dichroism spectra.

Representative commodity for five brassica vegetables based on the determination and dissipation of six pesticide residues

A Quick, Easy, Cheap, Effective, Rugged and Safe method for determination of thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, chlorpyrifos and lambda-cyhalothrin in five brassica vegetables by high performance liquid chromatography-mass spectrometry/mass spectrometry and gas chromatography-electron capture detector has been developed. The average recoveries of six pesticides in five brassica vegetables were in the range of 77.4%–117.4% with relative standard deviation of 3.7–10.8%. Residues of thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, chlorpyrifos and lambda-cyhalothrin in five brassica vegetables were studied with the developed method for the classification of crop group and selection of representative commodity of five brassica vegetables. Totally 48 open field trials on five brassica vegetables were conducted at two locations in two different seasons. The residue dynamics and final residues of the six pesticides at three preharvest intervals in different vegetables were compared. All six pesticides had the longest half-lives in cabbage (2.1–3.5 days). Residues of carbendazim (sum of thiophanate-methyl and carbendazim), metalaxyl, chlorpyrifos and lambda-cyhalothrin had similar trend in different brassica vegetables. The maximal concentrations of these pesticide residues were found in kale (0.28–10.9 mg kg^?1). Fluazifop-P-butyl residues were at low levels in all five brassica vegetables (<0.01–0.03 mg kg^?1). Cabbage, red cabbage, Brussels sprouts and kohlrabi had no significant difference in all six pesticide residues and could be classified in a subgroup of Head Brassicas. Cabbage should be selected as the representative commodity. Considering the highest residues in kale and its different morphology, kale should not be classified into the subgroup of Head Brassicas.     

Separation and Determination of Chemopreventive Phytochemicals of Flavonoids from Brassicaceae Plants

The main aim of this study was to develop a method for the isolation and determination of polyphenols—in particular, flavonoids present in various morphological parts of plants belonging to the cabbage family (Brassicaceae). Therefore, a procedure consisting of maceration, acid hydrolysis and measurement of the total antioxidant capacity of plant extracts (using DPPH assay) was conducted. Qualitative analysis was performed employing thin-layer chromatography (TLC), which was presented to be a suitable methodology for the separation and determination of chemopreventive phytochemicals from plants belonging to the cabbage family. The study involved the analysis of 25 vegetal samples, including radish, broccoli, Brussels sprouts, kale, canola, kohlrabi, cabbage, Chinese cabbage, red cabbage, pak choi and cauliflower. In addition, selected flavonoids content in free form and bonded to glycosides was determined by using an RP-UHPLC-ESI-MS/MS method.     

A comparative study of biochar,multiwalled carbon nanotubes and graphitized carbon black as QuEChERS absorbents for the rapid determination of six triazole fungicides by UPLC-MS/MS

A rapid, effective and sensitive method to quantitatively determine six fungicide residue was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). The target compounds were extracted by using acetonitrile and the sorbent used for clean-up in this modified QuEChERS analytical method were biochar, multiwalled carbon nanotubes (MWCNT) and graphitized carbon black (GCB). Results indicated that the MWCNT (10 mg) was the most effective sorbent in removing pigment. This method was validated on spinach, tomato, cucumber, celery, lettuce, rape, pakchoi, romaine lettuce and eggplant matrices spiked at three concentration levels of 0.01, 0.1 and 1 mg kg^?1. It exhibited recoveries between 73.1% and 118.2% with RSD values below 20%. Matrix-matched calibrations were performed with the coefficients of determination >0.9901 between concentration levels of 0.01–1 mg kg^?1. The limit of quantity (LOQ) for six pesticides ranged from 0.0036 to 0.011 mg kg^?1. The developed method was satisfactorily applied to determine pesticide residues in market vegetable samples.     

多壁碳纳米管-固相萃取分析有机磷农药残留

建立了多壁碳纳米管为吸附剂的固相萃取净化和火焰光度检测气相色谱法测定蔬菜中16种有机磷农药的方法.采用双柱双检测器进行定性和定量分析.建立了水相和有机相上样两种净化体系.水相上样时采用pH 5.0醋酸-醋酸钠缓冲体系,真空抽干除水,二氯甲烷为洗脱剂,只有9种农药的回收率>75%.对于正己烷溶解药物,丙酮-正己烷(5: 5,V/V)作洗脱剂的有机相净化体系,16种农药回收率均>75%.本研究提出的有机相上样净化体系用于黄瓜、卷心菜、韭菜、生姜和洋葱等样品的净化,效果良好,表明多壁碳纳米管具有较强的吸附和去除色素的能力,可以克服色素对测定的干扰.     

Simultaneous enantioselective determination of triazole fungicide difenoconazole and its main chiral metabolite in vegetables and soil by normal-phase high-performance liquid chromatography

Herein is reported, for the first time, a simple and highly sensitive chiral high-performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of difenoconazole stereoisomers and their hydroxylated metabolite difenoconazole alcohol (CGA-205375) enantiomers in vegetables and soil matrix. The separation of difenoconazole and CGA-205375 including their simultaneous enantioseparation was studied using four different polysaccharide-type chiral stationary phases (CSPs) in combination with n-hexane-polar organic alcohols mobile phase. Chiralcel OJ consisting of 25?% of cellulose tris(4-methylbenzoate) coated on wide-pore polysaccharide silica gel exhibited higher resolving ability compared to cellulose tris(3,5-dimethylphenylcarbamate) (Chiralcel OD) as well as to its similar amylose derivative (Chiralpak AD) CSPs for this particular set of chiral analytes. Baseline separation and simultaneous enantioseparation of difenoconazole and its metabolite CGA-205375 could be achieved under optimized separation conditions. Based on the established HPLC method, enantioselective analysis method for this fungicide and its main chiral metabolite in vegetables and soil matrix were developed and validated. Parameters including the matrix effect, linearity, precision, accuracy, and stability were evaluated. Under the optimal conditions, the mean recoveries from cucumber, tomato, and soil matrix ranged from 81.65 to 94.52?%, with relative standard deviations in the range of 1.05-8.32?% for all stereoisomers. Coefficients of determination R (2)?≥?0.998 were achieved for each enantiomer in the cucumber, tomato and soil matrix calibration curves within the range of 0.5-50?μg mL(-1). The limits of quantification for all enantiomers in three matrices were all below 0.1?μg mL(-1). The methodology was successfully applied for simultaneous enantioselective analysis of difenoconazole stereoisomers and their metabolite in the real samples, indicating its efficacy in investigating the environmental stereochemistry of difenoconazole in food and environmental matrix.     

Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry

The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI−) for chromafenozide. The limits of detection were below 0.6 μg kg⁻¹, while the limit of quantification did not exceed 2 μg kg⁻¹ in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg⁻¹). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4–13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.     

Studies on Amendment of Different Biopolymers in Sandy Loam and Their Effect on Germination,Seedling Growth of <Emphasis Type="Italic">Gossypium herbaceum</Emphasis> L.

Different biopolymers, agar, cellulose, alginate, psyllium gaur gum, and bacterial exopolysaccharide (EPS) powders were amended to check their efficacy in enhancing maximum water holding capacity (MWHC), permanent wilting point (PWP), and germination and seedling growth of the Gossypium herbaceum in a laboratory scale. The efficacy of all biopolymers for enhancement of MWHC, PWP, and growth was also analyzed by measuring organic carbon, organic matter, total nitrogen, respiration rate, and microflora in amended and control sandy loams. The range of concentrations (0.2–2%) of all biopolymers was incorporated in sandy loam containing pots. The soil without polymer was considered as control. The psyllium (0.6%) and bacterial EPS (1%) amended soil has 242 and 233% increase in MWHC and thus delaying in the permanent wilting point by 108 and 84 h at 37 °C, respectively, as compared to control. All biopolymers found to increase more or less MWHC, organic matter, total nitrogen, microflora, and PWP as compared to control. The psyllium and bacterial EPS show the highest increase organic matter, biomass, and microflora. The highest reduction in MWHC after 12 weeks were observed in cellulose, gaur gum, and alginate; besides, psyllium, bacterial EPS, and agar showed comparatively less reduction MWHC, i.e., 24% and 14.5%, respectively. The toxicity studies of biopolymer were carried out on earthworm (Eisenia foetida). It revealed their nontoxic nature. The biopolymer amendment in sandy loam can be an effective strategy to improved soil texture, fertility, and thereby crop yield.     

Human Health Risk Surveillance Through the Determination of Organochlorine Pesticides by High-Performance Liquid Chromatography in Water,Sediments, and Fish from the Chenab River,Pakistan

The current study assessed the spatiotemporal variations and human health surveillance associated with organochlorine pesticide (OCP) contamination in water, sediments, and fish from Chenab River, Pakistan. The OCP determinations were performed using high-performance liquid chromatography with a reverse-phase C18 column. The total OCP levels ranged from 13.33 to 274.59?ng/L in water, 4.63 to 239.11?ng/g in sediments, and 23.79 to 387.12?ng/g in fish species. The overall pattern of mean OCP concentrations followed the order as ΣDDTs?>?Σendosulfan?>?aldrin and OCP pollution pattern among the headworks were Khanki Barrage?>?Qadirabad Barrage?>?Trimmu Barrage?>?Marala Barrage in all three environmental matrixes during both seasons. The estimated daily intake (EDI) for ∑OCPs was found to be 22.44?ng/kg/day. The hazard ratios calculated to assess the carcinogenic risk indicated that the values for ∑DDT and aldrin at the 95th percentile concentrations were greater than one, indicating the probability of carcinogenic risk occurrence of one in million populations due to fish consumption. Therefore, these high levels of OCPs and carcinogenic risk through fish consumption highlight the needs of immediate elimination of OCPs from riverine environment of Chenab River and we recommend long-term monitoring-based freshwater ecological studies to be conducted in the study area.     

Appraisal of venomous metals in selected crops and vegetables from industrial areas of the Punjab Province

Due to the inadequate water sources, usually sewerage water and industrial effluents are being use for irrigation of the agricultural land around the industrial areas in Pakistan wherein crops and vegetables are cultivated. As untreated effluents contain heavy elements, toxic metals and organic pollutants that may find its way through food chain to general public and may cause health hazards. It is, therefore, mandatory to assess the toxic metals in such crops and vegetables. In this regard, samples of corn, millet, cabbage, spinach and potato were collected within the vicinity of industrial areas of the Faisalabad and Gujranwala regions. The food samples were analyzed using neutron activation analysis (NAA) technique. The highest concentration values of Arsenic (1.9 ± 0.1 μg/g) and Cobalt (0.85 ± 0.01 μg/g) were found in cabbage whereas Manganese (91.6 ± 0.2 μg/g), Antimony (0.15 ± 0.03 μg/g) and Selenium (1.1 ± 0.1 μg/g) were observed in spinach and Chromium (9.63 ± 1.3 μg/g) was found in millet crop. The observed concentrations of all the toxic and heavy metals in crops and vegetables are higher than those reported in the literature.     

Spectrophotometric Estimation of Carbaryl Residue in Some Home Garden Vegetables

Abstract

Residues of carbaryl (1-Naphthyl N-methly carbamate) were determined in the fruit and foliage of seven home garden vegetables by a spectrophotometric method. Residues at harvest averaged the following levels; cabbage (head, 0.0 ppm), cucumber (foliage 0.0 ppm; fruit, 0.05 ppm), garden bush beans (fruit, 0.0 ppm), Okra (foliage, 0.0 ppm; fruit, 0.01 ppm), pepper (foliage, 2.72 ppm; fruit, 0.9 ppm), squash (foliage, 6.55 ppm; fruit, 0.0 ppm), and tomato (foliage, 2.07 ppm; green fruit, 0.09 ppm; mature fruit, 0.03 opm). Foliage of the vegetables contained higher concentrations of the insecticide, in most cases, than did the fruits. Even with excessive applications, the carbaryl residues were found to be below the tolerance level established by EPA.     

Determination of macro and trace elements in canned marine products by inductively coupled plasma—optical emission spectrometry (ICP-OES) and ICP—mass spectrometry (ICP-MS)

This study determined the concentration of eight macroelements (Na, K, Mg, P, S, Ca, Fe, Zn) and nineteen trace elements (Li, Be, Cr, Mn, Co, Ni, V, Cu, Ga, Se, Rb, Sr, In, Sn, Cs, Ba, Tl, Bi, U) in commonly consumed canned marine products from South Korea. The samples were wet-digested using nitric acid and hydrogen peroxide by a microwave system and analyzed for macroelements using inductively coupled plasma—optical emission spectrometry (ICP-OES) and for trace elements by inductively coupled plasma—mass spectrometry (ICP-MS). The analytical methods were validated by the correlation coefficients, limits of detection and quantification, correlation variance, spiking recovery tests, and analyzing a NIST 1566?b oyster tissue certified reference material. The concentrations of macro and trace elements varied among the canned marine products. The macroelements were present in the order of Na?>?K?>?P?>?S> Mg?>?Ca?>?Fe?>?Zn. In general, the concentrations of macro and trace elements were within the specified limits of Food and Nutrition Board, Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives, and Ministry of Food and Drug Safety, Korea. The results suggest that the analyzed canned marine products are safe in terms of the analyzed elements and their consumption therefore does not cause any threat to human health.     

Assessment of the toxicity level of an industrial eco-system for its hazardous metals

Pakistan is an agricultural country, yet it is facing a serious threat due to the shortage of water resources and degradation of the agricultural land by the pollution of industrial effluents. A limited number of the current industries are equipped with proper operating treatment plants. Generally, the untreated effluents are disposed off to the open environment which is used for irrigation purposes. Therefore, vegetables and crops grown around the industrial areas is a major potential source of metal poisoning which pose a serious risk to the general public. Hence, study of the toxicity level in vegetables and crops is highly desirable. In this regard, systematic studies have been carried out to determine concentration levels of toxic elements in the samples of vegetables, crops, effluents and soil collected from the industrial areas of the Faisalabad. After processing, these samples were analyzed using neutron activation analysis and atomic absorption spectrometric techniques. The highest concentrations of toxic metals were observed for As (2.73 ± 0.34) in cabbage, Cd (1.5 ± 0.1), Ni (5.1 ± 0.9) and Pb (4.3 ± 0.2) in corn, Co (0.65 ± 0.02), and Sb (0.09 ± 0.01) in carrot, Cr (9.63 ± 1.3), Mn (46.5 ± 4.2) and Se (1.03 ± 0.1) in millet, Cu (11.3 ± 1.1) in tomato vegetables and crop samples. Although, the observed toxicity levels in vegetables and crop samples were higher than those grown in non-industrial areas, yet these toxicity levels are within the safe recommended limits.     

Simultaneous extraction and determination of fluoroquinolones,tetracyclines and sulfonamides antibiotics in soils using optimised solid phase extraction chromatography-tandem mass spectrometry

An analytical method was developed for the simultaneous extraction and determination of 18 fluoroquinolones (FQs), tetracyclines (TCs) and sulfonamides (SAs) antibiotics from soils using solid phase extraction and liquid chromatography-tandem mass spectrometry. The soils were extracted by different solvents with the help of mechanical shaking and ultrasonic treatment at 59?kHz, followed by a strong anion exchange (SAX) cartridge to clean up soil samples and a hydrophilic lipophilic balance (HLB) cartridge as enrichment. The method was evaluated by testing the following variables: extraction solvents, the type of SPE cartridges, solvent volumes, initial spiking levels and soil types (silty clay loam and clay loam soils). The soil extraction method was validated using these two types of soils, representing two typical agricultural soils in northern China. For 2?g soil, the extraction steps with the mixture of potassium phosphate buffer and acetonitrile (ACN) (1/1, v/v, pH 3.2) provided satisfactory recoveries. In the clay loam soil, the recoveries of all the compounds were from 56% to 89% at the spiking level of 50?µg?kg^?1 soil, and from 69% to 97% at the spiking level of 200?µg?kg^?1 soil, respectively. Recoveries in silty clay loam soil were similar to that in clay loam. The method was successfully employed using soil samples collected from a farmland and afforestion area irrigated with sewage in northern China. The result indicates that trace antibiotics in sewage may accumulate in soil irrigated by river water containing sewage.