首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
An ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for quantification of eight tranquillizers (chlorpromazine, imipramine hydrochloride, diazepam, nitrazepam, nordazepam, oxazepam, flurazepam, and haloperidol) in pork. Sample pretreatment consisted of extraction by acetonitrile, defatted by n-hexane, and further solid phase extraction by hydrophilic-lipophilic balance (HLB) extraction cartridges. The triple quadrupole mass spectrometer was operated in positive ion mode, and multiple reaction monitoring was used for drug quantification. The method was validated over the concentration ranges of 1.0 ~ 250 μg kg?1 for the eight tranquillizers. The calibrations were performed in sample matrices, and the interference effect of sample matrices on the ionization was effectively eliminated. Good linear relationship (R 2 > 0.99) was observed within the concentration range of 1.0–250 μg kg?1. The average recoveries of the eight tranquillizers spiked at three levels ranged from 63.7 to103.2 % with the relative standard deviation below 11.8 %. The limits of detection were between 0.06 and 0.30 μg kg?1, and the limits of quantification were between 0.2 and1.0 μg kg?1 for all analytes in pork. This validated method has been successfully used to quantify the concentration of the eight tranquillizers in pork samples.  相似文献   

2.
The natural co-occurrence of aflatoxins (AFs), ochratoxin A (OTA) and citrinin (CIT) in melon seed samples obtained from retailers and households in Ireland and the United Kingdom (UK) was evaluated. AFs and OTA were determined by HPLC with fluorescence detection while CIT was analysed by HPLC-MS/MS. AFB1 was detected in all (100%) samples (mean = 9.7 μg kg?1; range = 0.2–66.5 μg kg?1). Mean total AFs was 12.0 μg kg?1 (range = 0.3–82 μg kg?1). Commercially retailed samples showed a significantly higher AFB1 contamination (p < 0.05) than the household samples. OTA occurred in 3 (13.6%) samples, while 4 (18.2%) were contaminated with CIT at very low levels. In this study, 68% of the melon seed samples were contaminated above the 2 μg kg?1 EU limit for AFB1 in oilseeds. These results highlight the need for the development of strategies to reduce AF contamination in “egusi” for human consumption.  相似文献   

3.
A simple, fast, and efficient method was developed for simultaneous determination of 79 pesticides and 13 antibiotics compounds of different chemical classes of pesticides and antibiotics in honey samples by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). The sample preparation procedure includes homogenization with McIlvaine buffer 0.1 mol L?1 (pH 4), followed by extraction with acetonitrile and cleanup with florisil, using dispersive solid phase extraction (d-SPE). The proposed method was validated with good results, such as linearity (r 2?>?0.9901), normality, and independence of the evaluated data, as well as recoveries between 70 and 120 % with relative standard deviation (RSD) <20 % for most of the compounds spiked from 0.1 to 200 μg kg?1. The experimental method limits of detection and quantification were from 0.03 to 1.51 μg kg?1 and from 0.1 to 5 μg kg?1, respectively, for the pesticides. For the antibiotics, the decision limits (0.1 to 2 μg g?1) and the detection capacity (0.12 to 2.81 μg g?1) were below the maximum residue limits (MRLs) established for honey by the Brazilian and European legislation. The method was successfully applied to real samples from different botanical and geographic origins. From them, 44 % presented residues from 0.12 to 10 μg kg?1 of one or more analytes. The proposed method combines the advantages of a quick sample preparation step with the selectivity and sensitivity of the UHPLC-MS/MS and proved to be suitable for routine analyses.  相似文献   

4.
ABSTRACT

The determination of acrylamide in potato products, bakery products and coffee, and the human dietary exposure is reported. The method reported is based on a single extraction step with water, followed by the clean-up of the extract using solid phase extraction columns and finally, the determination of acrylamide using UPLC–MS/MS. The MS/MS detection was carried out using an ESI interface in positive ion mode. Internal calibration was used for the quantification of acrylamide, because of the suppression/enhancement matrix effects due to the complex nature of the samples. The method performance characteristics were determined after spiking blank samples. The mean recoveries in spiked coffee samples, potato chips, breakfast cereals and crispbread ranged from 93% to 99%, with RSDs lower than 5% for both repeatability and reproducibility conditions. The estimated limits of detection and quantification of the method were 10 and 32 μg kg?1, respectively. The method was used for monitoring acrylamide in 406 samples. Acrylamide amounts ranged from <32 to 2450 μg kg?1. A total of 360 samples (89%) were contaminated with acrylamide, but only 14% of the samples exceeded the benchmark levels of the EU legislation. Foods with the highest mean acrylamide amounts were potato crisps (642 μg kg?1), French fries (383 μg kg?1) and biscuits (353 μg kg?1). The mean and 95th percentile acrylamide exposures of adolescents in Cyprus were 0.8 and 1.8 μg kg?1 body weight per day, respectively. The estimated levels of dietary exposure to acrylamide are not of concern with respect to neurotoxicity. However, the margins of exposure (MOEs) indicate a concern for carcinogenicity. Potato fried products (45%), fine bakery ware (21%) and potato chips (14%) contributed the most to overall acrylamide exposure.  相似文献   

5.
A rapid and effective analytical method for determination of pydiflumetofen residues in some foods of plant and animal origin (grapes, tomatoes, wheat, pork, milk, and eggs) was developed using a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation procedure followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). Acetonitrile was served as the extraction solvent, and an octadecylsilane-dispersive solid-phase extraction (C18-dSPE) was used to cleanup the analyte, and then detected by UPLC–MS/MS. Pydiflumetofen was eluted within 3.0 min from the HSS T3 chromatography column connected to an electrospray ionization source in positive mode. The linearity of the method was excellent (R2?≥?0.992) in the pydiflumetofen concentration range of 10–1000 μg kg?1. The recoveries of spiked pydiflumetofen (10, 100, and 1000 μg kg?1) from the matrices were satisfactory, being between 72.0 and 110.3%, and all with relative standard deviation values of <?15.1%. The limit of quantification for pydiflumetofen was 10 μg kg?1. This study provides a method for the routine monitoring of pydiflumetofen.  相似文献   

6.
A fast and effective multiresidue method for the determination of 42 pesticides in golden berry was developed and validated. A modified QuEChERS method was established for sample preparation followed by ultra-high performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) determination with electrospray ionization in a triple quadrupole system. Validation results were satisfactory, since the method presented recoveries between 70 and 114 % with relative standard deviations (RSD) <20 % for blank samples spiked from 5 to 25 μg kg?1. The method limit of detection and limit of quantification were 1.5 and 5 μg kg?1 , respectively. Matrix effect ranged from ?32 to 218 % and was compensated using matrix-matched calibration. Method linearity was established from 2.5 to 100 μg kg?1 with r 2 ≥ 0.99. The proposed method combines the advantages of a simple and fast sample preparation step by a modified QuEChERS method with the high selectivity and sensitivity of the UHPLC-MS/MS system using selected reaction monitoring. The method was successfully applied to commercial samples, proving to be an efficient alternative for routine analysis. From the 16 analyzed samples, 13 presented residues of one or more pesticides (carbendazim, chlorpyrifos ethyl, dimethoate, propamocarb, and tebuconazole) in the concentration range of 2.0 to 55.6 μg kg?1.  相似文献   

7.
A highly sensitive ultra-performance liquid chromatographic method with diode-array detection was developed for residue determination of thiophanate methyl (TM), cyromazine (CYR), and their metabolites, carbendazim (MBC) and melamine (MEL). Edible fungi samples were treated using accelerated solvent extraction (ASE) followed by cleanup with solid-phase extraction (SPE). Under optimized conditions, good linearity was achieved with a correlation coefficient (r 2) of ≥0.9998. The limit of quantification was 0.36, 0.24, 0.4, and 0.5 μg kg?1 for MEL, CYR, MBC, and TM, respectively. The intra- and interday precisions (in terms of the relative standard deviation (RSD)) of the four analytes were in the range of 2.3–4.5 and 3.1–6.3 %, respectively. The recoveries for TM, MBC, CYR, and MEL in four edible fungi samples at three spiked levels of 0.6, 6, and 20 μg kg?1 for TM and MBC and 0.4, 4, and 20 μg kg?1 for CYR and MEL were in the range of 82–105 % with RSDs below 5.6 %. The proposed method can be used for the routine determination of CYR and MEL in edible fungi with high sensitivity and accuracy as well as low consumption of reagents.  相似文献   

8.
A simple method was developed for the simultaneous determination of glyphosate, its main degradation product (aminomethylphosphonic acid), and glufosinate in honey. Aqueous honey solutions were derivatised offline prior to direct analysis of the target analytes using online solid-phase extraction coupled to liquid chromatography-tandem mass spectrometry. Using the developed procedure, accuracies ranging from 95.2% to 105.3% were observed for all analytes at fortification levels of 5, 50, and 150 μg kg?1 with intra-day precisions ranging from 1.6% to 7.2%. The limit of quantitation (LOQ) was 1 μg kg?1 for each analyte. Two hundred honey samples were analysed for the three analytes with AMPA and glyphosate being most frequently detected (99.0% and 98.5% of samples tested, respectively). The concentrations of glyphosate were found to range from <1 to 49.8 μg kg?1 while those of its degradation product ranged from <1 to 50.1 μg kg?1. The ratio of glyphosate to AMPA was found to vary significantly amongst the samples where both analytes were present above the LOQ. Glufosinate was detected in 125 of 200 samples up to a maximum concentration of 33.0 μg kg?1.  相似文献   

9.
Acrylamide (ACR) is a potential carcinogen and is found in thermally processed foods such as potato chips, biscuits, baby foods, coffee, etc. In this paper, l-cysteine-capped Mn-doped ZnS quantum dots (QDs) as phosphorescent probes were used for the determination of ACR. This method based on quenching of the phosphorescence intensity of the QDs with the interaction of ACR. Room temperature phosphorescence (RTP) intensity of QDs was quenched rapidly upon the addition of the quencher. The quenching mechanism of Mn-doped ZnS QDs by ACR was dynamic and the quenching constant was found as 3 × 104 M?1. A linear response was observed from 2 to 20 μg mL?1 of ACR with a limit of detection of 0.56 μg mL?1. ACR was determined in all samples in the range of 24.3 to 453.2 g kg?1. The results showed that the proposed method is sensitive, selective, fast, and does not require a derivatization step.  相似文献   

10.
During 2012–2014, 170 samples of export quality raisins were collected from different vendors in Pakistan. The collected samples were analysed for the presence of aflatoxins (AFs) and Ochratoxin A (OTA) contamination using high-performance liquid chromatography technique. The limit of detection and limit of quantification of AFs/OTA were 0.12/0.10 and 0.36/0.30 µg kg?1, respectively. Only 5% of the samples were contaminated with AFs, ranging 0.15–2.58 µg kg?1 with a mean of 0.05 ± 0.26 µg kg?1. None of the raisin samples exhibited AFs contamination above the maximum limit (ML = 4 µg kg?1) as set by the European Union (EU). About 72% of the samples were contaminated with OTA, ranging 0.14–12.75 µg kg?1 with a mean of 2.10 ± 1.9 µg kg?1. However, in 95.3% of the tested samples, OTA level was lower than the ML of 10 µg kg?1 as regulated by the EU. Apparently, a strict and continuous monitoring plan, including regulatory limits, improves food safety and quality for all types of commodities.  相似文献   

11.
An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO4) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EU maximum residue limits (MRLs) for carrots, 10–50 μg kg?1, while the limit of quantification did exceed 10 μg kg?1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg?1), ranged from 66 to 111 % with relative standard deviations in the range of 2–15 % (n?=?3) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg?1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg?1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.  相似文献   

12.
A method for determination of ochratoxin A (OTA) in wines using a new-solid phase extraction clean-up procedure followed with ultra performance liquid chromatography (UHPLC)-Orbitrap MS based on two scan events (full-scan Fourier transform mass spectrometer [FTMS] and higher energy-induced collision dissociation[HCD] data-dependent MS/MS) in positive ionization mode has been developed. The limit of detection (LOD) was estimated at 0.46 μg l?1 for white wine, 0.53 and 0.54 μg l?1 for rosé and red wines, respectively. The limit of quantification (LOQ) was estimated at 1.57 μg l?1 in white wine, 1.77 and 1.81 μg l?1 in rosé and red wines. Recovery experiments were carried out with spiked samples at three concentration levels (2, 5 and 10 μg l?1). The OTA recoveries in spiked white wine samples varied from 69.6 % to 99.8 %, while the recoveries for rosé and red wine samples were in the range of 63.0–110.2 % and 63.6–103.2 %, respectively. Finally, based on the results, it is concluded that the combination of C18 cartridge with conventional particle packed columns and UHPLC LTQ-Orbitrap XL is an appropriate procedure for OTA analysis in wines.  相似文献   

13.
A sensitive high-performance liquid chromatography-UV (HPLC-UV) method, based on the Association of Analytical Communities (AOAC) Official method 2000.02, was developed and validated for the high-throughput analysis of patulin in in vitro experiments on apple puree agar medium (APAM). The importance of repeating the ethyl acetate extraction step at liquid-liquid extraction (LLE) was examined, as well as the extent of patulin degradation during the sodium carbonate clean-up. In addition to this alkaline clean-up, the efficiency of using an Oasis HLB or C18 cartridge as solid-phase extraction (SPE) clean-up was compared. This resulted in a two-step ethyl acetate LLE, followed by an Oasis HLB SPE clean-up, without alkaline clean-up conditions. The method was fully validated for APAM, cloudy apple juice, and apple puree. Average patulin recoveries at levels of 100, 500, and 1000 μg kg?1 of APAM varied between 95 and 113 % over 3 independent days, with an interday precision (RSDR) of 5 to 10 %. Recovery experiments carried out with the spiked apple juice (at 50 μg kg?1) and apple puree (10 μg kg?1) showed average recovery rates laying between 80–101 % (RSDR?=?12 %) and 77–100 % (RSDR?=?9 %), respectively. This method offered a detection limit of 3–4 μg kg?1 and a quantification limit of 5–8 μg kg?1 for APAM, apple juice, and puree.  相似文献   

14.
The 3-monochloro-1,2-propandiol (3-MCPD) levels in soy sauces which contained hydrolysed vegetable protein were evaluated for the Bulgarian market. For analysis of 3-MCPD, a gas chromatography–mass spectrometry (GC-MS) method was applied with a linear range of 0.03–2.00 μg mL?1 and a limit of detection (LOD) of 2.3 μg kg?1 and a limit of quantification (LOQ) of 3.4 μg kg?1. At these levels, the standard deviation was 5.1%, with recoveries between 81% and 102%. The method was applied to the analysis of 21 samples of soy sauce from the Bulgarian market. Results ranged from 3.7 to 185.6 μg kg?1. Soy sauces produced from hydrolysed soy protein contained higher levels of 3-MCPD than naturally fermented sauces. In 38.4% of samples of Bulgarian origin, the 3-MCPD content was above the EU limit of 20 μg kg?1. In all analysed samples, 33.3% had a 3-MCPD content above the EU limit.  相似文献   

15.
Ultrahigh-performance liquid chromatography tandem mass spectrometry with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF) derivatization was developed for simultaneous determination of 20 free amino acids in Chinese jujube date. The MS/MS conditions, choice of mobile phase, the extraction process, and matrix effects were studied with a view to a method of optimization. The limits of detection for measurement of the amino acids ranged from 0.8 to 600.0 μg L?1. The correlation coefficients (r2?≥?0.9947) indicated good correlation between the concentrations of amino acids and the peak areas for the CNBF-derivatives. Recoveries for samples spiked at 25.0, 50.0, and 100.0 mg kg?1 ranged from 66.3 to 106.6 % (except tryptophan spiked at 25.0 and 50.0 mg kg?1, which provided recoveries of 61.2 and 60.4 %, and tyrosine spiked at three different concentrations, which provided recoveries of 54.8–58.6 %), with relative standard deviation values of less than 9.1 %.  相似文献   

16.
A green, simple and sensitive method was developed for the analysis of volatile carboxylic acids (VFAs) and perfluorocarboxylic acids (PFCAs) in food packaging materials. The acidic compounds in food packaging materials were first extracted by gas purge microsyringe extraction (GP–MSE) with 1.0 mL 0.1 mol·L?1 NaOH solution, then the analytes were dispersive liquid-liquid microextracted (DLLME) by 50 μL chloroform as extraction solvent and 200 μL acetonitrile as dispersive solvent. The 2-(5-Benzoacridine) ethyl-p-toluenesulfonate (BAETS) with excellent fluorescence property was applied to enhance the high performance liquid chromatography (HPLC) sensitivity. The obtained recoveries for the VFAs ranged from 92.0 to 101 %. The method LODs calculated at a signal-to-noise ratio (S/N) of 3 were in the range of 0.80–3.40 μg·kg?1, while the LOQs calculated at S/N of 10 were in the range of 2.5–10.2 μg·kg?1. All compounds were in good linearity with concentration coefficients of higher than 0.997. Perfluorooctanoic acid (PFOA) was found in all of the 15 kinds of samples analyzed with concentrations ranging from 4.86–7.56 μg·kg?1. Acetic acid, butyric acid, and caprylic acid were found in half of the samples analyzed. The other analytes were also found in more than 30 % samples with concentrations varied between 3.96 and 293 μg·kg?1.  相似文献   

17.
The aim of this study was to investigate the presence of tetracycline residues in pasteurised cow’s milk using high-performance liquid chromatography coupled with UV/VIS detection to determine the exposure of Brazilian’s population to antibiotic residues. One hundred samples collected from the State of Paraná, Brazil, were analysed. Three of these samples were contaminated at the following concentrations: 121.8 µg·kg?1 for oxytetracycline, 93.5 µg·kg?1 for tetracycline and 134.6 µg·kg?1 for chlortetracycline (61.6 µg·kg?1) and doxycycline (73.0 µg·kg?1). The median tetracycline residue concentration found in the samples was 42.3 µg·kg?1, and the estimated daily intake (EDI) was 0.05 µg Kg?1 bw day?1 in Brazil. These results demonstrate that the occurrence of tetracycline in Brazilian milk was low (3%) and only for 2% above the maximum residue limit, so the risk to the population from the presence of these residues in milk was low (<1% of the acceptable daily intake).  相似文献   

18.
Subcritical water extraction followed by solid-phase extraction and ultra-high performance liquid chromatography coupled with tandem mass spectrometry detection is reported for the first time for the determination of 6 trichothecenes (deoxynivalenol, deoxynivalenol-3-glucoside, 3-acetyl-deoxynivalenol, 15-acetyl-deoxynivalenol, HT-2 toxin, and T-2 toxin) from different cereals. Water with 1% formic acid was used as the extraction solvent followed by a solid-phase extraction clean-up, achieving good performance with acceptable extraction recoveries, method detection limits between 0.05 μg kg?1 and 4.0 μg kg?1, and method quantification limits between 0.4 μg kg?1 and 20 μg kg?1. The use of water as the extraction solvent allowed a selective extraction affording low matrix effect levels and the detection and quantification of natural target trichothecenes at very low concentration levels. This extraction method was applied to different cereals, a pseudocereal and an oilseed sample, of which maize, millet, and oat were contaminated by at least one trichothecene.  相似文献   

19.
Ultra high-performance liquid chromatography-electrospray ionization-mass spectrometry (UHPLC/ESI/MS) methodology was adapted for identification and quantification of tocopherols and tocotrienols in vegetable oils with no derivatization or sample preparation steps. The UHPLC analysis was performed using a C18 column and mobile phase composed of methanol: water: ammonium hydroxide (99:1:0.1 v/v/v) and isopropanol. A single mass spectrometer with electrospray on negative mode was used as a detector for tocopherols and tocotrienols. The samples were diluted in isopropanol. The limit of quantification for tocopherols was 0.006 μg mL?1, and the linear range was 0.006 to 0.01 μg mL?1; for tocotrienols, the limit of quantification was 0.002 μg mL?1, and the linear range of analysis was 0.002 to 0.003 μg mL?1. The correlation coefficients were higher than 0.99, indicating that the method has suitable linearity. The methodology has proven to be precise, reproducible, and robust for the parameters studied.  相似文献   

20.
A novel procedure, dispersive solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed for the determination of eugenol in aquatic products (shrimp, crab, and carp). Aquatic products were extracted with acetonitrile and primarily purified by dispersive solid-phase extraction with graphitized carbon black as absorbent. The pretreated acetonitrile extract was detected by UHPLC-MS/MS. UHPLC was carried out on Dikma Endeavorsil C18 (30 mm × 2.1 mm, 1.8 μm) column eluted by methanol and water (80:20 v/v) at a rate of 0.30 mL min?1. Tandem mass spectrometry was performed by electrospray ionization in negative ion mode to identify and quantify eugenol during multiple reaction monitoring. Under optimized analytical conditions, the matrix-matched spiked calibration sample demonstrates good linearity between 5.0 and 500.0 μg kg?1 with a linear regression coefficient of 0.9996. The average recovery of eugenol from aquatic products is 95.3–103.4% at spiked levels between 5 and 50 μg kg?1 with a relative standard deviation (n = 6) less than 5.4%. The limits of detection and quantification for eugenol were calculated to be 1.47 and 4.91 μg kg?1, respectively. In comparison with those reported, the proposed method has advantages in low detection limit, high recovery, and short analysis time, meeting the requirements for the determination of trace eugenol residue in aquatic products.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号