共查询到20条相似文献,搜索用时 15 毫秒
1.
A sensitive and reliable method has been developed and validated for the determination of chloramphenicol in poultry and swine liver using SPE and ultra-performance liquid chromatography (UPLC)/MS/MS. The liver samples were extracted with ethyl acetate, defatted with n-hexane, and further cleaned up using SPE cartridges with polymeric sorbent. An Acquity BEH C18 column was used for gradient UPLC separation, with water and acetonitrile as the mobile phase. The multiple reaction monitoring mode was used for two precursor-product ion transitions for chloramphenicol and one for the internal standard. The method was validated at 0.1, 0.3, and 1.0 microg/kg. Mean recoveries from fortified samples ranged from 95.5 to 106.7% with an RSD of 12.2%. The method LOD was < 0.02 microg/kg. 相似文献
2.
Pozo OJ Barreda M Sancho JV Hernández F Ll Lliberia J Cortés MA Bagó B 《Analytical and bioanalytical chemistry》2007,389(6):1765-1771
Ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC–MS–MS) has been used for screening and quantification
of 32 pesticides and metabolites in two fruit matrices. The compounds investigated belonged to different chemical families
of insecticides, acaricides, fungicides, and herbicides; several metabolites were also included. Quantification was conducted
using matrix-matched standards calibration; response was a linear function of concentration in the range tested (10–500 ng
mL−1). The method was validated with blank samples of lemon and raisin spiked at 0.01 and 0.1 mg kg−1, and recoveries were satisfactory, between 70 and 110%, for most of the pesticides tested and relative standard deviations
were below 15% (n = 5 at each spiking level). Excellent sensitivity resulted in limits of detection for all compounds well below 0.01 mg kg−1, with the limit of quantification being validated at 0.01 mg kg−1. The UPLC system generates narrow peaks (approx. 5 s), thus increasing peak height and improving sensitivity. This improved
separation efficiency facilitates adequate resolution not only of the analytes but also of matrix interferences compared with
conventional HPLC. The method developed could also resolve some geometric isomers. The main advantage of this approach is
the high sample throughput achieved because of the short analysis time, which enables satisfactory separation of all the compounds
in less than 5 min per sample. 相似文献
3.
The purified extract of propolis is used as a traditional remedy for the treatment of several diseases. Its beneficial activities are mainly attributed to the polyphenolic fraction. Nevertheless, propolis can cause allergic dermatitis and the sensitization rate in humans is increasing significantly mainly in younger subjects. The aim of this study was to develop and validate a selective and sensitive ultra‐performance liquid chromatography tandem mass spectrometry analysis (UPLC/MS/MS) for the evaluation of the amount of caffeic acid and its esters with allergenic action in raw propolis samples and commercial formulations. The separation was carried out on a 1.7 μm C18 BEH Shield column and the detection performed by means of electrospray ionization in negative ion mode with multiple reaction monitoring. The confirmation of formulae of the precursor and product ions was accomplished by injection into a high‐resolution system (FTICR‐MS) using accurate mass measurements. The error was below 1.4 ppm.The range of the standard curves was 0.5–10 μg/mL and dihydrocaffeic acid was used as internal standard (IS). The lower limit of detection (LLOD) for 3‐methyl‐2‐butenyl‐ (3M2B), 3‐methyl‐3‐butenyl‐ (3M3B), 2‐methyl‐2‐butenyl‐ (2M2B), benzyl‐ (CABE), phenylethylcaffeic acid (CAPE) and for caffeic acid (CA) and the IS was 0.1 and 0.3 μg/mL, respectively. The recoveries were in the range 96–104% and the intra‐ and inter‐day precisions were within 6.2%. In the European (n = 8) and Asiatic (n = 3) propolis the most abundant allergens were CABE>3M2B>CAPE>3M3B>CA>2M2B. These compounds were not found in the red (n = 1) and green (n = 1) Brazilian propolis. Hydroalcoholic extracts (n = 6) and tablets (n = 6) were analyzed by the proposed UPLC/MS/MS method. The results showed that in the commercial products CABE, 3M2B, CAPE and 3M3B were also the most abundant. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
4.
A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCI, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g. 相似文献
5.
A fast and accurate ultra-performance liquid chromatography coupled with electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI-Q-TOF-MS/MS) method was developed for the separation and structural elucidation of fluorescent carbon nanoparticles (CNP). The CNP was synthesised from microwave-assisted pyrolysis of citric acid (CA) and 1,2-ethylenediamine (EDA). By using UPLC separation, the CNP product was well separated into ten fractions within 4.0 min. Based on high-accuracy MS and MS/MS analyses, the CNP species were revealed to display six kinds of chemical formulas, including (C10H20N4O5)n, (C8H12N2O5)n, (C16H22N4O9)n, (C6H8O7)n, (C14H18N2O11)n, and (C14H16N2O10)n. In particular, our study revealed for the first time that the CNP species exist as supramolecular clusters with their individual monomers units linked together through non-covalent bonding forces. These findings clearly indicated the usefulness of UPLC-ESI-Q-TOF-MS/MS in identifying the chemical composition of CNP product. It is anticipated that our proposed methodology can be applied to study the structure-property relationships of CNP, facilitating in the production of CNP with desirable spectral features. 相似文献
6.
Yadav M Rao R Kurani H Rathod J Patel R Singhal P Shrivastav PS 《Journal of chromatographic science》2010,48(10):811-818
A sensitive and high throughput ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method has been developed for the determination of pramipexole, a dopamine agonist, in human plasma. Sample preparation involved liquid-liquid extraction of pramipexole and ranitidine as the internal standard (IS) in ethyl acetate from 100 μL human plasma. The chromatographic separation is achieved on a Waters Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) analytical column using an isocratic mobile phase, consisting of 10 mM ammonium formate (pH 7.50)-acetonitrile (15:85, v/v), at a flow-rate of 0.5 mL/min. The precursor → product ion transition for pramipexole (m/z 212.1 → 153.0) and IS (m/z 315.0 → 176.1) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) and positive ion mode. The method was validated over a wide dynamic concentration range of 20-4020 pg/mL. Matrix effect is assessed by post-column infusion experiment and the process efficiency were 91.9% and 85.7% for pramipexole and IS, respectively. The method is rugged and rapid with a total run time of 1.5 min and is applied to a bioequivalence study of 0.25 mg PPX tablet formulation in 30 healthy Indian male subjects under fasting condition. 相似文献
7.
固相萃取-超高压液相色谱-串联质谱同时分析环境水样中四环素类和喹诺酮类抗生素 总被引:5,自引:0,他引:5
应用固相萃取及超高压液相色谱-质谱联用技术,建立了环境水样中4种四环素类和6种喹诺酮类抗生素的同时分析方法。样品经HLB固相萃取柱富集、净化后用甲醇洗脱,以超高压液相色谱-串联质谱仪多反应监测(MRM)离子模式定性、定量分析。以河水和海水为基质,卡巴氧为替代物进行回收率评价,4种四环素类抗生素在加标质量浓度分别为20.0 ng/L和100.0 ng/L时的回收率为94.0%~117.0%,相对标准偏差为2.0%~9.7%(n=4),方法的检出限均为20.0 ng/L;6种喹诺酮类抗生素在加标质量浓度分别为5.0 ng/L和20.0 ng/L时的回收率为63.6%~93.9%,相对标准偏差为1.6%~8.1%(n=4),方法的检出限为0.4 ng/L。结果表明,所建立的方法可成功地应用于近岸海域表层环境水样中目标抗生素残留的分析。 相似文献
8.
Montoro EP González RR Frenich AG Torres ME Vidal JL 《Rapid communications in mass spectrometry : RCM》2007,21(22):3585-3592
A rapid multiresidue method for the analysis of more than 40 herbicides (such as simazine, terbuthylazine and diuron) in waters has been developed and validated by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS). Prior to chromatographic determination, the samples were extracted using a solid-phase extraction procedure. The analysis was performed on an Acquity UPLC BEH C(18) column using a gradient elution profile and a mobile phase consisting of methanol and an aqueous solution of formic acid (0.01%). Other chromatographic and MS/MS parameters were optimised in order to improve selectivity and sensitivity of the analytes. The analytes were detected using electrospray ionisation (ESI)-MS/MS in positive ion mode with multiple reaction monitoring (MRM), optimising parameters such as voltage cone, capillary voltage, source and desolvation temperature, and desolvation and cone gas flow. The optimised method provides a rapid separation (less than 10 min) of the selected herbicides in the assayed matrices, and it was validated by the analysis of spiked blank matrix samples. Good linearity was obtained and the repeatability of the method was less than 20% for the lowest calibration point. The limits of detection ranged from 0.002 to 0.02 microg/L, and the limits of quantification from 0.005 to 0.05 microg/L, which were below the values specified by the European Union. Finally, the method was successfully applied to real environmental samples from Andalusia (southern Spain). Terbuthylazine, simazine, atrazine desisopropyl and desethyl terbuthylazine were the herbicides most frequently found in water samples. 相似文献
9.
An improved method was validated for the determination of acrylamide in foods using ultra-performance liquid chromatography (UPLC) coupled to eletrospray ionization tandem mass spectrometry (MS/MS) in the present study. This improved method supplies a rapid quantitative procedure of acrylamide with a run time of only 3 min. Results showed a good repeatability (RSD< or =4.5%) with 50, 100, 250, 500 and 1000 microg/kg spiked concentrations in potato crisps in within-day (n=5) and day-to-day (n=10) precision tests. Meanwhile, good recoveries (81.6-99.0%) were obtained with the same spiked concentrations in acrylamide-free cereal samples (n=3). The excellent method validation data and proficiency test results (Z-score: -0.1) of the official Food Analysis Performance Assessment Scheme (FAPAS) suggested that the present quantitative method could be applied for rapid determination of acrylamide in many investigations. 相似文献
10.
An ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UPLC-ESI-MS(n)) has been developed for structural characterization and identification of multi-constituents in Yiqing Capsule, a well-known combined herbal remedy prepared from the extract mixtures of Rhizoma Coptidis, Radix et Rhizoma Rhei and Radix Scutellariae. The UPLC analysis was performed on an Agilent ZorBax SB-C(18) column (4.6 mm×50 mm, 1.8 μm) and gradient elution of 0.1% formic acid solution and acetonitrile in 16 min. Based on their retention times and mass spectra in comparison with the data from standards or references, a total of 29 compounds including 3 phenolic acids and 4 anthraquinones from Radix et Rhizoma Rhei, 8 alkaloids from Rhizoma Coptidis and 14 flavonoids from Radix Scutellariae were unambiguously identified or tentatively characterized in the complex system. The MS data and fragmentation information of two isomers of feruloylquinic acid were first reported in Radix et Rhizoma Rhei and in Yiqing Capsules. This study is expected to be accepted as an effective and reliable pattern for comprehensive and systematic characterization of this commonly used Chinese herbal preparation. 相似文献
11.
Shibata M Hashi S Nakanishi H Masuda S Katsura T Yano I 《Biomedical chromatography : BMC》2012,26(12):1519-1528
The purpose of this study was to develop an ultra‐performance liquid chromatography tandem mass spectrometry (UPLC‐MS/MS) method of 22 antiepileptics for routine therapeutic monitoring. The antiepileptics used in the analyses were carbamazepine, carbamazepine‐10,11‐epoxide, clobazam, N‐desmethylclobazam, clonazepam, diazepam, N‐desmethyldiazepam, ethosuximide, felbamate, gabapentin, lamotrigine, levetiracetam, N‐desmethylmesuximide, nitrazepam, phenobarbital, phenytoin, primidone, tiagabine, topiramate, valproic acid, vigabatrin and zonisamide. After protein precipitation of 50 μL plasma with methanol, the supernatant was diluted with water or was evaporated to dryness and reconstituted with mobile phase in the case of benzodiazepines. Separation was achieved on an Acquity UPLC BEH C18 column with a gradient mobile phase of 10 mm ammonium acetate containing 0.1% formic acid and methanol at a flow rate of 0.4 mL/min. An Acquity TQD instrument in multiple reaction monitoring mode with ion mode switching was used for detection. All antiepileptics were detected and quantified within 10 min, with no endogenous interference. All the calibration curves showed good linearity in the therapeutic range (r2 < 0.99). The precision and accuracy values for intra‐ and inter‐assays were within ±15% except for phenobarbital and tiagabine. A good correlation was observed between the concentration of clinical samples measured by the new method described here and the conventional methods. The values of carbamazepine and phenytoin by UPLC‐MS/MS were lower than those detected by the immunoassays, which might be caused by the cross‐reaction of antibodies with their metabolites. In conclusion, we developed a simple and selective UPLC‐MS/MS method suitable for routine therapeutic monitoring of antiepileptics. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
12.
Şeyda Kıvrak 《液相色谱法及相关技术杂志》2016,39(19-20):847-851
A rapid and sensitive ultra-performance liquid chromatography–tandem mass spectrometry method with electrospray ionization (UPLC–ESI–MS/MS) for analysis of B-group vitamins in honey has been presented. Aim of this study is the characterization of different types of Turkish honeys according to B-group vitamins. Vitamins were determined in 17 different types of Turkish honey samples by UPLC–ESI–MS/MS. Heather honey samples were distinguished among the studied honeys with the richest vitamin content with 286.10?mg/kg, and it is followed by sunflower honey and thyme honey with the total vitamin contents of 206.01 and 163.27?mg/kg, respectively. The presence of vitamin B1 (thiamine), vitamin B2 (riboflavin), vitamin B3 (nicotinamide, B3N and nicotinic acid, B3H), vitamin B6 (pyridoxine), and vitamin B9 (folic acid) was detected in all the honey samples analyzed. Moreover, vitamin B5 (pantothenic acid) was observed in most of them. Vitamin B12 (cyanocobalamin) and vitamin B7 (biotine) were not detected in the studied honey samples. Turkish honey samples showed efficacious vitamin content for the consumers. 相似文献
13.
We report here an ultra-performance liquid chromatography coupled with tandem mass spectrometric (MS/MS) method for the simultaneous quantitation of multiclass veterinary drugs in egg. The analysis of the target compounds, including 7 tetracyclines and 4 types of quinolones, may be accomplished in 15 min of total run time. The egg was extracted with ethylenediaminetetraacetic acid-Mcllvaine buffer solution and further purified using a polymer-based Oasis HLB solid-phase extraction cartridge. A C18 column was used to separate the analytes followed by MS/MS using an electrospray ion source. The overall average recoveries of the analytes based on matrix-fortified calibration ranged from 71 to 112% with acceptable relative standard deviations of <20% for 6 trials. For all of the target compounds, the limits of quantitation ranged between 0.02 and 4.29 microg/kg. The proposed method is sufficiently sensitive and highly selective. 相似文献
14.
A simple method for the determination of some anthelmintic drugs and phenylbutazone residues in milk and muscle was developed. Following a fast and easy extraction and evaporation procedure, the extract was injected into an ultra performance liquid chromatography system coupled to a single stage Orbitrap detector. The high mass resolution of 50,000 full width at half maximum and corresponding narrow mass windows permitted a very selective and sensitive detection of analytes without requiring fragmentation of the observed [M+H]+ or [M+Na]+ ions. This eliminated some difficulties which have plagued the analysis of compounds belonging to the group of avermectins. The analytical method was validated according to the EU commission decision for Orbitrap based, but also for more traditional tandem mass spectrometry based detection and quantification. Equal repeatability but significantly higher sensitivity for critical compounds (avermectins) was obtained for the Orbitrap based detection. A result of this study was the conclusion that analytes with poor fragmentation properties (e.g. sodium-cationized molecules) can be more easily quantified by single stage high resolution mass spectrometry than by tandem mass spectrometry. 相似文献
15.
超高效液相色谱/高分辨飞行时间质谱法同时检测乳制品中19种抗生素 总被引:2,自引:0,他引:2
利用超高效液相色谱/高分辨飞行时间质谱结合数据库建立了乳制品中19种抗生素的分析方法。样品依次经过乙腈和酸化乙腈处理后,冷冻离心浓缩,经超高效液相色谱分离,正离子扫描模式下,在10 min内对19种抗生素进行分离和检测,质量浓度在10~500或15~1000 μg/L范围内具有良好的线性关系,检出限为3~5 μg/L,平均回收率为68.4%~96.7%。加标样品的筛查结果表明,保留时间偏差不大于0.1 min,质量偏差小于5 mDa,同位素峰形匹配度不低于87.4%, 19种加标抗生素被全部检测出来,且大部分抗生素获得很高的鉴定评分。对购自本地超市的40余份乳制品进行了筛查分析,未检出阳性样品。该分析方法具有前处理简单、分析速度快、灵敏度高、质量精确度高的特点,可应用于乳制品中抗生素的快速筛查。 相似文献
16.
Proctor Kathryn Petrie Bruce Barden Ruth Arnot Tom Kasprzyk-Hordern Barbara 《Analytical and bioanalytical chemistry》2019,411(27):7061-7086
Analytical and Bioanalytical Chemistry - This paper presents a new multi-residue method for the quantification of more than 142 anthropogenic compounds of emerging concern (CECs) in various... 相似文献
17.
A method based on ultra-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry for the determination of six thyreostatic drugs in thyroid tissue has been optimised and validated in accordance with the Decision 2002/657/EC. Samples are extracted with methanol and the extracts cleaned-up on silica cartridges. The recoveries range from 40% for 6-phenyl-2-thiouracil to 79% for 2-thiouracil. Quantification is carried out with blank tissue samples spiked with the analytes in the range 25-500 microg kg(-1). 5,6-Dimethyl-2-thiouracil is used as internal standard. CCalpha and CCbeta are in the ranges 4.3-16.1 microg kg(-1) and 8.7-20.7 microg kg(-1), respectively. Accuracy, expressed as percentage of error, is lower than 6% and relative standard deviation in reproducibility conditions falls between 5.6 and 10.3%. Nowadays, the proposed method is routinely implemented in the laboratory of the Agència de Salut Pública de Barcelona and allows processing of up to 20 samples per day. 相似文献
18.
Simultaneous determination of 24 sulfonamide residues in meat by ultra-performance liquid chromatography tandem mass spectrometry 总被引:2,自引:0,他引:2
The present study used the liquid extraction pretreatment method and developed an ultra-performance liquid chromatography triple quadrupole tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of 24 kinds of sulfonamide residues in meat. The meat samples were homogenized, extracted and deproteinized by acetonitrile, defatted by n-hexane, and further liquid-liquid extracted by ethyl acetate. All of 24 sulfonamide residues were simultaneously separated and determined by UPLC-MS/MS within 15 min. The sulfonamide residues were monitored via the ESI(+) ionization method and quantified by six-channel multiple reaction monitoring (MRM). The calibrations were performed in sample matrixes by the isotope dilution method and the interference effect of sample matrixes on the ionization was effectively eliminated. Good linear relationship (R(2)=0.991-0.999) was observed within the concentration range of 0.2-50 microg/kg. Satisfied recoveries (67.8-113.9%) of all the sulfonamides were demonstrated in different standard-spiked levels except sulfanitran (SNT). The analytical category, separation speed, selectivity, sensitivity and repeatability of sulfonamides using UPLC-MS/MS were significantly improved compared to other analytical methods. Quantitative results of 240 meat samples demonstrated that the present method has a convenient operation and good practicability, which can be applied to the quantitative analysis of a large number of samples. 相似文献
19.
Mark Cronly Patrice Behan Barry Foley Edward Malone Liam Regan 《Journal of chromatography. A》2009,1216(46):8101-8109
A rapid confirmatory method has been developed and validated for the simultaneous identification, confirmation and quantitation of 11 nitroimidazoles in eggs by liquid chromatography tandem mass spectrometry (LC–MS/MS). The method is validated in accordance with Commission Decision 2002/657/EC and is capable of analysing metronidazole (MNZ), dimetridazole (DMZ), ronidazole (RNZ), ipronidazole (IPZ) and their hydroxy metabolites MNZ-OH, HMMNI (hydroxymethyl, methyl nitroimidazole), IPZ-OH. The method is also capable of analysing carnidazole (CRZ), ornidazole (ORZ), tinidazole (TNZ) and ternidazole (TRZ). MNZ, DMZ and RNZ have been assigned a recommended level (RL) of 3 μg kg−1 by the Community Reference Laboratory (CRL) in Berlin. The developed method described in this study is easily able to detect all the nitroimidazole compounds investigated at this level and below. Egg samples are extracted with acetonitrile, and NaCl is added to help remove matrix contaminants. The acetonitrile extract undergoes a liquid–liquid wash step with hexane; it is then evaporated and reconstituted in mobile phase. The reconstituted samples are analysed by liquid chromatography tandem mass spectrometry (LC–MS/MS). The decision limits (CCα) range from 0.33 to 1.26 μg kg−1 and the detection capabilities (CCβ), range from 0.56 to 2.15 μg kg−1. The results of the inter-assay study, which was performed by fortifying hen egg samples (n = 18) on three separate days, show the accuracy calculated for the various analytes to range between 87.2 and 106.2%. The precision of the method, expressed as %CV values for the inter-assay variation of each analyte at the three levels of fortification (3, 4.5 and 6.0 μg kg−1), ranged between 3.7 and 11.3%. A Day 4 analysis was carried out to examine species variances in eggs from different birds such as duck and quail and investigating differences in various battery and free range hen eggs. 相似文献
20.
Strategy for metabonomics research based on high-performance liquid chromatography and liquid chromatography coupled with tandem mass spectrometry 总被引:12,自引:0,他引:12
Yang J Xu G Zheng Y Kong H Wang C Zhao X Pang T 《Journal of chromatography. A》2005,1084(1-2):214-221
Metabonomics, the study of metabolites and their roles in various disease states, is a novel methodology arising from the post-genomics era. This methodology has been applied in many fields. Current metabonomic practice has relied on mass spectrometry (MS), gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance (NMR) to analyze metabolites. In this study, a strategy was developed for applying high-performance liquid chromatography (HPLC) and LC-MS-MS to metabonomics research. One of the key problems to be solved in this strategy is to match the peaks between the chromatograms. A peak alignment algorithm has been developed to match the chromatograms before the pattern recognition. As an application example, the strategy described above was applied to metabonomics research on liver diseases, and the false-positive result of live cancer diagnosis from the hepatocirrhosis and hepatitis diseases was effectively reduced to 7.40%. Based on the pattern recognition, several potential biomarkers were found and further identified by the following LC-MS-MS experiments. The structures of eight potential biomarkers were given for distinguishing the liver cancer from the hepatocirrhosis and hepatitis diseases. 相似文献