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1.
《Analytical letters》2012,45(14):2317-2331
The genus Stellaria (Caryophyllaceae) presents widely distributed plants often used in traditional medicine. Flavonoids are highly active plant secondary metabolites that may be involved in some of the effects of Stellaria plants. In this study, two new high-performance liquid chromatography–electrospray ionization tandem mass spectrometry (HPLC–ESI-MS-MS) methods were developed for the determination of flavonoids and isoflavonoids in plant material. The separations were performed on a reverse-phase C18 column with gradient elution using methanol and water with 0.5% acetic acid as the mobile phase. Multiple reaction monitoring was used for the tandem mass spectrometry detection and the two most intensive transitions were chosen for the identification of each analyte. The limits of detection and the limits of quantification were between 0.2 and 15.0 ng/mL and 0.6 and 50.0 ng/mL. The developed methods were successfully used for the analyses of four representatives of the genus Stellaria. All the studied herbs contained luteolin and its 7-O-glycosides, naringenin, kaempferol, quercetin, its glycoside rutin, apigenin, and its 7-O-glycoside. One coumarin, scopoletin, was also found. Isoflavones were primarily represented by genistein, genistin, and ononin. Some of the analytes were detected for the first time in Stellaria sp. The findings support that these methods are suitable for analyses of plant material.  相似文献   

2.
Milk adulteration is a concern in many countries, including Brazil. There are many compounds used as adulterants, including cheese whey, a by-product of cheese. Recently, we have developed a proteomic-like technique for separation and characterization of caseinomacropeptide using liquid chromatography coupled to mass spectrometry with electrospray ionization. Caseinomacropeptide is important because it can be used as marker when cheese whey adulteration is performed in bovine milk. Furthermore, it is difficult to establish reference values for caseinomacropeptide levels because of the variation of milk composition. The aim of this study was to verify the average value for caseinomacropeptide present in bovine raw milk collected by Federal Inspection Service from five regions of Brazil (north, northwest, west central, south, southeast). Survey sampling was divided into two stages: first one, a data set 1 (regional sampling) was collected only from the south during a year. This data sampling was used to estimate the data set 2 (national sampling). A largest extreme value was suggested as a model for caseinomacropeptide distributions for national sampling. The data set showed 2.52?mg?L?1 as the mean and 4.80?mg?L?1 for the standard deviation based on a sampling size of 170?units collected across Brazil. The findings are useful to understand the presence of caseinomacropeptide, especially when no adulteration or the absence of good practices is present.  相似文献   

3.
ABSTRACT

A sensitive and selective method was developed to determine pesticides in carrots by gas chromatography–mass spectrometry following the development of an optimized extraction procedure. The method was validated for 30 organochlorine pesticides for gas chromatography with electron capture detection obtaining limit of detection from 0.18 to 0.92?µg/kg except for cis- and trans-permenthrin. Twenty-six carrot samples were analyzed and six pesticides were detected. The results compared with the accepted maximum residue levels in correlation to crop origin.  相似文献   

4.
Cyclosporine, tacrolimus, sirolimus, and everolimus are commonly used immunosuppressants following organ transplantation. Their monitoring is used to determine the optimal dose for therapeutic effectiveness and minimize toxicity. High-performance liquid chromatographic–tandem mass spectrometry with positive electrospray ionization and multiple reaction monitoring mode was validated for the determination of cyclosporine A, tacrolimus, sirolimus, and everolimus in whole blood. A C18 analytical column was employed with a gradient elution of pH 4.0 aqueous 10?mmol/L ammonium acetate and acetonitrile. For the pretreatment of whole blood, simple protein precipitation was used with methanol:zinc sulfate. The calibration curves were linear from 20.0 to 1000?ng/mL for cyclosporine A, 1.0 to 50?ng/mL for tacrolimus and sirolimus, and 1.0 to 30?ng/mL for everolimus. The intra-assay precision and inter-assay precision were less than 15%. The method provides reliable and reproducible results according to the linearity, precision, accuracy, recovery, and matrix effects. The method has been introduced to routine clinical practice in Slovakia for the determination of immunosuppressants in patients after kidney transplantation.  相似文献   

5.
A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric method (LC-MS-MS) for the determination of eupatilin in human plasma has been developed. Eupatilin and an internal standard; (S)-N-(3-{3-fluoro-4-[6-(1-methyl-1H-tetrazol-5-yl)-pyridine-3-yl]-phenyl}-2-oxo-oxazolidin-5-ylmethyl)-acetamide (DA-7867) were extracted from human plasma by liquid-liquid extractionand analyzed on a phenyl-hexyl column using the mobile phase: acetonitrile-ammonium formate (10 mM, pH 3.0) (60:40, /). Analytes were detected using electrospray ionization-tandem mass spectrometry in multiple-reaction monitoring mode. The calibration curve was linear (r = 0.999) over the concentration range: 1.00–500 ng mL–1 with a lower limit of quantification of 1.0 ng mL–1 using a 100 L plasma sample. The precision (CV%) of this assay ranged: 2.4–7.0%, relative error: –7.0 to +2.0%. Recoveries of eupatilin ranged: 64.3–65.0%, with that of DA-7867 (internal standard) being 87.0 ± 5.3%.  相似文献   

6.
An ultrahigh-performance liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous determination of sterigmatocystin, verruculogen, enniatin A, fusarenon-X, fumonisins B1, B2, B3, aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, 3-acetyldeoxynivalenol, 5-acetyldeoxynivalenol, and zearalenone. The mycotoxins were extracted and cleaned up using a multitoxin column, separated on a C18 column, and then detected on a triple-quadrupole mass spectrometer. The limits of detection and quantification ranged within 0.2–2?µg/kg and 1–10?µg/kg, respectively. The recoveries ranged from 70.8 to 118.4%, with relative standard deviations below 15%. The method was used to analyze 80 samples obtained from Shandong Province in China. Fifty-eight samples were contaminated with 10 mycotoxins at concentrations ranging from 1.4 to 6566.1?µg/kg. Some samples exceeded the maximum limits in China and in European regulations for mycotoxins in unprocessed maize.  相似文献   

7.
《Analytical letters》2012,45(13):1979-1987
Liquid chromatography with tandem mass spectrometry was used for the determination of nitrofurantoin, nitrofurazone, furazolidone, and furaltadone in chicken feed. The nitrofurans were extracted with phosphate buffer (pH 7) and sodium chloride. Proteins and lipids were removed with acetonitrile and hexane before purification with ethyl acetate, dilution in 1:1 acetonitrile-5 millimolar ammonium acetate at pH 7.3, and filtration prior to analysis. The limits of detection were 1.69, 1.74, 2.01, and 1.45 microgram per kilogram for nitrofurantoin, nitrofurazone, furazolidone, and furaltadone, respectively. The mean recoveries were between 84.6 and 110.6 percent. The method was employed to determine nitrofurans in chicken feed.  相似文献   

8.
《Analytical letters》2012,45(10):1634-1649
A selective method for the determination of fourteen nitroimidazoles and their hydroxy-metabolites in honey was developed based on improved molecularly imprinted solid-phase extraction followed by liquid chromatography–tandem mass spectrometry. The separation of analytes was performed on a C18 column using a mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water with gradient elution. The method was suitable for metronidazole, hydroxymetronidazole, dimetridazole, ronidazole, hydroxydimetridazole, ipronidazole, hydroxyipronidazole, carnidazole, menidazole, nimorazole, ornidazole, secnidazole, ternidazole, and tinidazole. The procedure was evaluated according to EU Commission Decision 2002/657/EC requirements by determining linearity, specificity, recovery, repeatability, within-laboratory reproducibility, decision limit, detection capability, matrix effects, and stability. The method determined nitroimidazoles and their hydroxy-metabolites below the recommended concentration level of 3 µg kg?1. The decision limits and detection capabilities ranged from 0.110 µg kg?1 to 0.387 µg kg?1 and from 0.179 µg kg?1 to 0.508 µg kg?1, respectively. The results from stability tests indicated that all analyzed nitroimidazoles were stable in honey stored at 4°C for at least 28 weeks and that elevated temperature and exposure to light exposure accelerated their degradation. The method was successfully applied to the analysis of a wide variety of honey samples.  相似文献   

9.
High-performance liquid chromatography coupled with high-resolution mass spectrometry was used for the determination of polyphenols in Lycium barbarum leaves. Twenty compounds extracted by methanol–water were tentatively identified that included chlorogenic acids, flavonoids, and phenolic acids. Neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C were identified in Chinese cultivated L. barbarum leaves for the first time. Caffeic acid and isoquercitrin were also present. The concentrations of these compounds in L. barbarum leaves were determined. The results showed that all analytes had linear calibration relationships with limits of detection from 0.318 to 3.35?ng mL?1. The polyphenols and flavonoids in L. barbarum leaves provided strong 2,2-diphenyl-1-picrylhydrazyl radical-scavenging capacity (IC50 of 23.1?±?0.4 to 26.0?±?0.4?µg mL?1). This method is suitable for the determination of polyphenols in L. barbarum leaves, which provide polyphenols with suitable antioxidant activity.  相似文献   

10.
《Analytical letters》2012,45(6):934-943
Infant formula provides a good source of fructooligosaccharides, which are considered to be functional ingredients of food due to their positive effects on gastrointestinal function. This study presents a simple and specific ultra-high performance liquid chromatography–tandem mass spectrometry method for the ultrasensitive determination of three fructooligosaccharides in infant formula. The analytes were extracted using acetonitrile-water solutions. The compounds were separated with an amide column by gradient elution using acetonitrile and water as mobile phases. The identification and quantification were achieved by using electrospray ionization tandem mass spectrometry in negative ion mode with multiple reaction monitoring. Accuracy, precision, limits of quantification, and limits of detection of the method were obtained. Under the optimal conditions, all calibration curves for fructooligosaccharides targets showed good linearity (R2 ≥ 0.998). The limits of detection and quantification were below 0.82 and 2.74 ng mL?1, respectively. The recoveries of the method ranged from 98.5% to 104.4%. To the knowledge of the authors, this is the first quantitative determination of fructooligosaccharides in infant formula by ultra-high performance liquid chromatography–tandem mass spectrometry. The method may be suitable for the determination of trace concentrations of fructooligosaccharides in other food.  相似文献   

11.
5-hydroxymethyl-2′-deoxycytidine (5-hmdC), which plays important roles in the epigenetic remodeling in mammals, has been recently determined in plant genomes at trace concentrations. In this study, a method for the sensitive, specific, and rapid assessment of 5-hmdC in rice is reported using high-performance liquid chromatography–tandem mass spectrometry (HPLC–tandem MS) with isotope dilution. The recovery of this method was from 75.6% to 81.3% for 5-hmdC and the intra- and inter-day precision values were within 5.81%. The quantification limit for 5-hmdC was 5.0?pM. Genomic DNA from rice was extracted and enzymatically digested for nucleotides for the HPLC–tandem MS assay. The 5-hmdC levels were 1.32?±?0.08, 1.64?±?0.12, and 1.98?±?0.07 modifications per million nucleosides in the Shengdao-18, Shengxiang-145, and Jindao-263 rice cultivars. The application of HPLC–tandem MS for 5-hmdC demonstrated its presence in the genomic DNA of rice and is useful in further studying the role of modified cytosine in the epigenetic regulation of rice.  相似文献   

12.
《Analytical letters》2012,45(14):2307-2316
A facile method based on liquid chromatography coupled with triple quadrupole mass spectrometry was established to determine floridoside and isofloridoside in red algae. Correlation coefficients of the calibration curves were larger than 0.9989, indicated good linearity. Detection limits of floridoside and isofloridoside were 0.05 and 0.20 ng/mL, respectively, and the limits of quantification were 0.1 and 0.4 ng/mL. The recoveries varied from 75.7% to 76.8%, and relative standard deviations of inter-day and intra-day precision were lower than 8.5% (n = 5). The effects of sea level variations in the intertidal zone on the osmotic role of floridoside and isofloridoside concentrations in seven red algae were investigated. It was shown that algae that inhabit higher levels in the intertidal zone contained higher concentrations of floridoside and isofloridoside. The results suggest that the presence of direct sun, exposure time, and temperature influenced to the concentrations of floridoside and isofloridoside due to the osmotic pressure adjustments.  相似文献   

13.
Using high-performance liquid chromatography combined with tandem mass spectrometric detection, an approach has been developed for the determination of the most stable nerve agent biomarker, methylphosphonic acid, in human blood plasma. The proposed method is based on the derivatization of methylphosphonic acid with p-bromophenacyl bromide. The optimization of conditions for human plasma sample preparation, mass spectrometric detection conditions, and gradient elution program has been performed. The proposed approach has demonstrated satisfactory reproducibility and selectivity of the determination; the limit of detection for methylphosphonic acid in human plasma was 3 ng mL–1.  相似文献   

14.
An analytical method was established to simultaneously quantify flonicamid and its metabolites 4-trifluoromethylnicotinic acid (TFNA), N-(4-trifluoromethylnicotinoyl) glycine (TFNG), and 4-trifluoromethylnicotinamide (TFNA-AM) in tea using orthogonal experimental design and liquid chromatography–tandem mass spectrometry (LC–MS/MS). Residues were extracted from the samples with acetonitrile containing 1% acetic acid and were purified with graphitized carbon black. The linearity of the method was excellent in the concentration range of 0.01–10?µg/mL, producing correlation coefficients greater than 0.996 for the target compounds. The limits of detection and quantification of all analytes in tea were 0.0013–0.013?mg/kg and 0.004–0.040?mg/kg, respectively. The average recoveries of flonicamid, TFNA, TFNG, and TFNA-AM ranged from 75.14 to 92.72%, with intra- and interday relative standard deviations of 1.07–9.75%. The proposed method was successfully applied to the terminal residue determination of flonicamid and its metabolites in dry tea processed from three field trials’ fresh samples. The determined total terminal residue concentrations of flonicamid 10?days after the last application at all three sites were below the maximum residue limit (MRL) set by the European Union (0.1?mg/kg) and the residues in all samples were lower than the MRL established by the United States Environmental Protection Agency (EPA) (8?mg/kg). This method may be used to meet the requirements for the determination of flonicamid and its metabolites that could provide guidance for establishing a MRL for flonicamid in tea in China.  相似文献   

15.
An indirect method is described for determination of phytate in human urine. The method is based on hydrolysis of the phytate and determination of myo-inositol, one of the hydrolysis products. Chromatographic separations were performed on an Aminex HPX-87C column with Milli-Q water as mobile phase; 5 mM ammonium acetate was added post-column. The detector counted positive ions by monitoring m/z=198, which corresponds to the adduct of myo-inositol with the ammonium cation. The relative standard deviations obtained for standards containing 0.5, 1, and 1.5 mg L–1 phytate were 4.1, 3.0, and 2.7% respectively (n=5). The limit of detection was 60 g L–1. Different urine samples were analyzed both by this method and by an alternative analytical method based on GC–MS. The results from both methods were comparable.  相似文献   

16.
Antibiotics are often used in bee-keeping to control European and American foulbrood. The broad spectrum antibiotic chloramphenicol (CAP) was used for curative purposes in veterinary medicine, but is now forbidden in numerous countries, although still used in south-east Asia. A liquid-chromatographic method with tandem mass spectrometric detection (LC–MS–MS) has been developed for analysis of sub-g kg–1 residues of chloramphenicol in honey. Results from full validation of the procedure and analysis of 75 honey samples obtained commercially in Switzerland are presented. These show the method is satisfactory and useful for monitoring chloramphenicol residues in honey.  相似文献   

17.
The objective of this study was to develop an analytical method based on ultrasonic-assisted dispersive liquid–liquid microextraction (DLLME) for the determination of 19 pesticides in Shengmaiyin and its resulting crude drugs Ophiopogon japonicas and Codonopis pilosula. The target compounds were qualitatively and quantitatively studied via ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) operated in multiple reaction-monitoring modes. The UHPLC–MS/MS conditions were optimized to complete chromatographic separation in 9 min. The correlation coefficient was higher than 0.993 for each pesticide. Average recoveries of the 19 compounds from different fortified samples ranged between 81 and 108 % with inter-RSD values below 13 %. The limits of quantification (LOQs) for 19 compounds were in the range of 0.0075–0.81 μg kg?1. Recovery LOQs of the DLLME method were compared with the routine QuEChERS method, and the results showed that the proposed method is very simple, rapid, and sensitive. This makes it a more applicable method for monitoring multiple classes of pesticides in traditional Chinese medicine.  相似文献   

18.
In this paper, a sensitive accurate method for the determination of heterocyclic aromatic amines (HAAs) in cigarette smoke has been developed and validated using solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry. A calibration curve was obtained with representative cigarette smoke using the standard addition method to compensate for matrix effects because the smoke of different cigarettes shows similar matrix effects. With this method, the accuracy of the method can be improved using a common analog of HAAs, which will greatly reduce the expense of using an isotope-labeled internal standard. Validation results showed that the method has high sensitivity (quantification limits of 0.08–0.56 ng cig?1), good reproducibility (RSD 6.37–9.31 %) and satisfactory recoveries (81.0–111 %). With this method, the emissions of HAAs in 30 commercial cigarette samples were analyzed and compared.  相似文献   

19.
Zhao  Ge  Wang  Sheng  Fu  Yufeng  Yu  Jingjing  Wang  Bing  Xie  Fuwei  Xie  Jianping 《Chromatographia》2014,77(11):813-820

In this paper, a sensitive accurate method for the determination of heterocyclic aromatic amines (HAAs) in cigarette smoke has been developed and validated using solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry. A calibration curve was obtained with representative cigarette smoke using the standard addition method to compensate for matrix effects because the smoke of different cigarettes shows similar matrix effects. With this method, the accuracy of the method can be improved using a common analog of HAAs, which will greatly reduce the expense of using an isotope-labeled internal standard. Validation results showed that the method has high sensitivity (quantification limits of 0.08–0.56 ng cig−1), good reproducibility (RSD 6.37–9.31 %) and satisfactory recoveries (81.0–111 %). With this method, the emissions of HAAs in 30 commercial cigarette samples were analyzed and compared.

  相似文献   

20.
《Analytical letters》2012,45(17):3208-3218
Abstract

A method for the detection of microcystins (microcystin LR, RR, and YR) in cyanobacteria by supercritical fluid extraction (SFE) and liquid chromatography‐mass spectrometry (LC/MS) has been developed. Supercritical fluids for the analytical extraction of nonvolatile, higher molecular weight compound, and microcystins from cyanobacteria were investigated. The microcystins included in this study are sparsely soluble in neat supercritical fluid CO2. However, the microcystins was successfully extracted with a ternary mixture (90% CO2, 9.5% methanol, 0.5% water) at 40°C and 250 atm. The polar carbon dioxide‐aqueous methanol fluid system gave high extraction efficiency for the extraction of the polar microcystins from cyanobacteria. The microcystins were determined by liquid chromatography‐tandem mass spectrometry (LC/MS/MS).  相似文献   

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