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1.
Yan Liang Jie Sun Lin Xie An Kang Yuan Xie Wei-Dong Chen Hua Lv Guang-Ji Wang 《Chromatographia》2007,66(3-4):165-170
A sensitive and specific liquid chromatographic method with electrospray ionization mass spectrometry (LC–ESI-MS) has been
developed and validated for identification and quantification of mitiglinide in human urine. A simple liquid–liquid extraction
procedure was followed by separation on a C18 column with gradient elution, and detection using a single-quadrupole mass spectrometer in selected-ion-monitoring (SIM)
mode. The method was tested using six different batches of urine. Linearity was established for the mitiglinide concentrations
in the range 0.005–1.0 μg mL−1, with a coefficient of determination (r) of 0.9998 and good back-calculated accuracy and precision. Intra- and inter-day precision (as RSD, %) was below 10% and
accuracy for mitiglinide ranged from 85 to 115%. The lower limit of quantification was reproducible at 0.002 μg mL−1 for 500 μL urine. The proposed method enables unambiguous identification and quantification of mitiglinide in pre-clinical
and clinical studies. 相似文献
2.
A rapid ultra-high-performance liquid chromatographic–tandem mass spectrometric (UHPLC–MS–MS) method has been developed for
rapid screening and quantitative analysis of sulfonate derivatives (SDs) in commercial white peony root. Separation was performed
on an Agilent Zorbax Eclipse Plus-C18 column by gradient elution with acetonitrile–0.1% (v/v) formic acid as the mobile phase. In-source fragmentation was used to generate the characteristic fragment ion at m/z 259 and to screen for nine SDs. Detection of these SDs was further performed in multiple reaction monitoring (MRM) mode to
improve sensitivity and to quantify the two SDs paeoniflorin sulfonate and benzoylpaeoniflorin sulfonate. The method was validated
for specificity, linearity, limits of detection and quantification, precision, accuracy, and matrix effects. Nine commercial
white peony root samples were examined by use of this method, which revealed great variety in the paeoniflorin sulfonate and
benzoylpaeoniflorin sulfonate content. 相似文献
3.
A liquid chromatography-tandem mass spectrometric (LC-MS-MS) method was developed and validated for the determination of the anticholinergic and antimuscarinc drug propiverine and eight of its metabolites in serum, urine, faeces and different tissue samples of rats. Samples containing propiverine and its metabolites in serum and urine and in the supernatants of faeces and tissue homogenates were extracted and cleaned up using an automated solid phase extraction (SPE) method. An external calibration was used. The analytes were measured employing the multiple reaction monitoring mode (MRM). A sufficient response over the range of 10-1000 ng/ml was demonstrated. The lower limit of quantification of the nine substances was 10 ng/ml. The presented method is suitable for pharmacokinetic or toxicokinetic studies. To look for additional unknown metabolites, the LC-MS-MS system operated in the precursor ion mode using typical product ions of propiverine and of its metabolites. With the help of the chromatographic behaviour and typical fragment ions of the unknown metabolites, it was possible to elucidate their structure. Five until now unknown metabolites were found in the urine and faeces samples. However, without reference substances, a quantification of these analytes was not possible. 相似文献
4.
5.
This paper presents a general screening method, based on liquid chromatography/mass spectrometry (LC/MS), for the simultaneous
detection in human urine of 72 xenobiotics (21 diuretics, 16 synthetic glucocorticoids, 17 beta-adrenergic drugs, 10 stimulants,
5 anti-oestrogens and 3 anabolic steroids), excreted free or as glucuro-conjugates in urine. Although the method has been
specifically designed and evaluated in view of its potential application to anti-doping analyses, it can also be effective
in other areas of analytical toxicology. Sample preparation was based on two liquid/liquid separation steps (performed at
alkaline and at acid pH, respectively) of hydrolyzed human urine, and then an assay by LC/MS-MS in positive and negative ionization
mode using an electrospray ionization source (ESI) and multiple reaction monitoring (MRM) as the acquisition mode. The overall
time needed for an LC run was less than 15 minutes. All compounds showed good reproducibility in terms of both the retention
times (CV%<1) and the relative abundances of the diagnostic transitions (CV%<10). The limits of detection (LOD) were in the
range of 1–50 ng/mL for glucocorticoids, anti-oestrogens and steroids, and 50–500 ng/mL for diuretics, beta-adrenergic drugs
and stimulants, thus satisfying the minimum required performance limits (MRPL) set by the World Anti-Doping Agency (WADA)
for the accredited anti-doping laboratories. 相似文献
6.
Wohlfarth A Toepfner N Hermanns-Clausen M Auwärter V 《Analytical and bioanalytical chemistry》2011,400(3):737-746
An LC-MS/MS method for the determination of the atypic neuroleptic clozapine and its two main metabolites norclozapine and
clozapine-N-oxide has been developed and validated for serum and urine. After addition of d4-clozapine as deuterated internal standard
a fast single-step liquid–liquid extraction under alkaline conditions and with ethyl acetate as organic solvent followed.
The analytes were chromatographically separated on a Synergi Polar RP column using gradient elution with 1 mM ammonium formate
and methanol. Data acquisition was performed on a QTrap 2000 tandem mass spectrometer in multiple reaction monitoring mode
with positive electrospray ionization. Two transitions were monitored for each analyte in order to fulfill the established
identification criteria. The validation included the determination of the limits of quantification (1.0 ng/mL for all analytes
in serum and 2.0 ng/mL for all analytes in urine), assessment of matrix effects (77% to 92% in serum, 21 to 78% in urine)
and the determination of extraction efficiencies (52% to 85% for serum, 59% to 88% for urine) and accuracy data. Imprecision
was <10%, only the quantification of norclozapine in urine yielded higher relative standard deviations (11.2% and 15.7%).
Bias values were below ±10%. Dilution of samples had no impact on the correctness for clozapine and norclozapine in both matrices
and for clozapine-N-oxide in serum. For quantification of clozapine-N-oxide in urine a calibration with diluted calibrators has to be used. Calibration curves were measured from the LOQ up to
2,000 ng/mL and proved to be linear over the whole range with regression coefficients higher than 0.98. The method was finally
applied to several clinical serum and urine samples and a cerebro-spinal fluid sample of an intoxicated 13-month-old girl. 相似文献
7.
Kacinko SL Concheiro-Guisan M Shakleya DM Huestis MA 《Analytical and bioanalytical chemistry》2008,392(5):903-911
A liquid chromatography–tandem mass spectrometry method for the simultaneous quantification of buprenorphine (BUP), norbuprenorphine
(NBUP), buprenorphine glucuronide (BUP-Gluc), and norbuprenorphine glucuronide (NBUP-Gluc) in human urine was developed and
fully validated. Extensive endogenous and exogenous interferences were evaluated and limits of quantification were identified
empirically. Analytical ranges were 5–1,000 ng/mL for BUP and BUP-Gluc and 25–1,000 ng/mL for NBUP and NBUP-Gluc. Intra-assay
and interassay imprecision were less than 17% and recovery was 93–116%. Analytes were stable at room temperature, at 4 °C,
and for three freeze–thaw cycles. This accurate and precise assay has sufficient sensitivity and specificity for urine analysis
of specimens collected from individuals treated with BUP for opioid dependence. 相似文献
8.
This paper reports a novel approach for the detection, confirmation, and quantification of 15 selected pyrethroid pesticides,
including pyrethins, and two metabolites of dithiocarbamates in foods by ultra-performance liquid chromatography–tandem mass
spectrometry (UPLC–MS–MS). The proposed method makes use of a modified QuEChERS (quick, easy, cheap, effective, rugged, and
safe) procedure that combines isolation of the pesticides and sample cleanup in a single step. Analysis of pyrethroids and
dithiocarbamate metabolites was performed by UPLC–MS–MS operated with electrospray and atmospheric pressure chemical ionization,
respectively. Two specific precursor–product ion transitions were acquired per target compound in multiple reaction monitoring
(MRM) mode. Such acquisition achieved the minimum number of identification points according to European Commission (EC) document
no. SANCO/10684/2009, thus fulfilling the EC point system requirement for identification of contaminants in samples. The method
was validated with a variety of food samples. Calibration curves were linear and covered from 1 to 800 μg kg−1 in the sample for all target compounds. Average recoveries, measured at mass fractions of 10 and 100 μg kg−1 for pyrethroids and 5 and 50 μg kg−1 for dithiocarbamate metabolites, were in the range of 70–120% for all target compounds with relative standard deviations
below 20%. Method limits of quantification (MLOQ) were 10 μg kg−1 and 5 μg kg−1 for pyrethroids and dithiocarbamate metabolites, respectively. The method has been successfully applied to the analysis of
600 food samples in the course of the first Hong Kong total diet study with pyrethroids and metabolites of dithiocarbamates
being the pesticides determined. 相似文献
9.
Leonardo S. Teixeira Iram M. Mundim Weidson C. Souza Douglas R. Ramos Karine B. Bellorio Fernanda G. Marques Kênnia R. Rezende 《Chromatographia》2009,69(Z2):149-156
A fast, sensitive and specific liquid chromatography-mass spectrometry method has been developed for quantification of digoxin
in human plasma. The method was optimized to bioequivalence studies aiming higher sensitivity and selectivity than previously
published methods, in addition to shorter run time allowing high-throughput sample analyses from volunteers. Chromatographic
separation was achieved by an RP-18e column hyphenated to an API 5000 mass spectrometer system set at negative electrospray
ionization and operating in the MRM mode. Calibration curve was linear over a wide range of concentration (50.0–6000.0 pg mL−1), with the lower limit of quantification at 50.0 pg mL−1 and without interfering peaks at the retention time of digoxin (2.09 min). Dexamethasone was used as internal standard and
samples were cleaned up by liquid-liquid extraction obtaining a mean recovery of 73.8%. Validation results confirmed inter-batch
accuracy (−8.66 to 5.78%), precision (4.1–10.6%) and stability, in accordance with the U.S. Food and Drug Administration and
the Brazilian National Health Surveillance Agency guidelines. The developed analytical method could be successfully applied
to a single oral dose (0.25 mg), one-way, randomized, two-sequence, crossover bioequivalence study validating, up to date,
the fastest analysis and the most sensitive and specific method already published for digoxin quantification. 相似文献
10.
高效液相色谱-离子阱质谱法测定尿液中β2-受体激动剂及β-受体阻断剂 总被引:1,自引:0,他引:1
建立了尿液中23种β2-受体激动剂及5种β-受体阻断剂的高效液相色谱-离子阱质谱(HPLC-IT-MS)测定方法。尿液样品采用冷冻高速离心沉淀蛋白,上清液过ExtrelutTM硅藻土柱,用乙酸乙酯洗脱后,洗脱液经旋转蒸发仪浓缩并复溶待测。HPLC分离采用AtlantisT3-150 mm色谱柱,以甲醇和含0.1%甲酸的水溶液为流动相梯度洗脱,IT-MS采用电喷雾离子源在多反应离子监测模式下测定。定量分析选择9种经过氘代同位素标记的β2-受体激动剂为内标。各化合物的线性范围为0.005~0.16 mg/L,尿液中的检出限均能达到0.2 μg/L。空白尿液样品中不同加标水平的回收率为57.1%~127.1%,相对标准偏差为1.1%~31.1%。该方法简便快速,灵敏度高,适用于人或动物尿液中23种β2-受体激动剂及5种β-受体阻断剂的定性和定量分析。 相似文献
11.
Authors developed a simple, sensitive, selective, rapid, rugged, and reproducible liquid chromatography–tandem mass spectrometry
method for the quantification of eletriptan (EP) in human plasma using naratriptan (NP) as an internal standard (IS). Chromatographic
separation was performed on Ascentis Express C18, 50 × 4.6 mm, 2.7 μm column. Mobile phase was composed of 0.1% formic acid:
methanol (40:60 v/v), with 0.5 mL/min flow rate. Drug and IS were extracted by liquid–liquid extraction. EP and NP were detected with proton
adducts at m/z 383.2→84.3 and 336.2→97.8 in multiple reaction monitoring (MRM) positive mode, respectively. The method was validated with
the correlation coefficients of (r
2) ≥ 0.9963 over a linear concentration range of 0.5–250.0 ng/mL. This method demonstrated intra- and inter-day precision within
1.4–9.2% and 4.4–5.5% and accuracy within 96.8–103% and 98.5–99.8% for EP. This method is successfully applied in the bioequivalence
study of 24 human volunteers. 相似文献
12.
Summary A method was developed for the separation and quantification of the warfare nerve agent sarin (O-isopropylmethylphosphonoflouridate), its metabolite methylphosphonic acid, the anti nerve agent drug pyridostigmine bromide
(PB;3-dimethylaminocarbonyloxy-N-methyl pyridinium bromide) and its metaboliteN-methyl-3-hydroxypyridinium bromide in rat plasma and urine. The method involved using solid phase extraction and high performance
liquid chromatography (HPLC) with reversed phase C18 column, and UV detection at 280 nm. The compounds were separated using gradient of 1% to 55% acetonitrile in 0.1% triflouroacetic
acid water solution (pH 3.20) at flow rate of 0.9 ml/min in a period of 15 min. The retention times ranged from 4.4–12.1 min.
The limits of detection were 50 ng mL−1 for PB andN-methyl-3-hydroxypyridinium bromide, and 10 μg mL−1 for sarin and methylphosphonic acid, while limits of quantitation were between 100 ng mL−1–12 μg mL−1. Average percentage recovery of five spiked samples from plasma were 84.6±8.4, 86.5±9.0, 76.4±8.5, 81.3±8.2, and from urine
78.5±7.9, 76.4±7.8, 74.4±8.4, 80.6±6.8 for sarin, methylphosphonic acid, pyridostigmine bromide andN-methyl-3-hydroxypyridinium bromide, respectively. This method was applied to analyze the above chemicals and metabolites
following combined administration in rats. 相似文献
13.
A novel method using liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry in the
negative selected ion monitoring mode has been developed and validated for rapid simultaneous determination of triptolide
and tripdiolide in the extract of Tripterygium wilfordii Hook. f. The molecular ions m/z [M–H]− 359 and 375 were selected for the quantification in selected ion monitoring mode for triptolide and tripdiolide. Standard
calibration curve was linear over the concentration range of 0.12–24 and 0.15–30 μg mL−1 for triptolide and tripdiolide. The relative standard deviations of intra- and inter-day were in the range of 4.7–9.9 and
8.9–12.6%. The average recoveries were between 96.4 and 104.6%. The limits of quantitation were 2.0 × 10−3 and 2.5 × 10−3 μg mL−1 for triptolide and tripdiolide. 相似文献
14.
Saito T Fukushima T Yui Y Miyazaki S Nakamoto A Namera A Inokuchi S 《Analytical and bioanalytical chemistry》2011,400(1):25-31
We present a method based on monolitic spin column extraction and gas chromatography–mass spectrometry as an analytical method
for screening diquat (DQ), paraquat (PQ), and fenitrothion in serum and urine. This method is useful for clinical and forensic
toxicological analyses. Recovery of DQ, PQ, and fenitrothion from serum and urine, spiked at concentrations between 0.1, 2.5,
20, and 45 μg/ml, ranged from 51.3% to 106.1%. Relative standard deviation percentages were between 3.3% and 14.8%. Detection
and quantitation limits for serum and urine were 0.025 and 0.05 μg/ml, respectively, for DQ, 0.1 and 0.1 μg/ml, respectively,
for PQ, and 0.025 and 0.05 μg/ml, respectively, for fenitrothion. Therefore, these compounds can be detected and quantified
in the case of acute poisoning. 相似文献
15.
A. Vonaparti E. Lyris I. Panderi M. Koupparis C. Georgakopoulos 《Analytical and bioanalytical chemistry》2009,395(5):1403-1410
In equine sport, salicylic acid is prohibited with a threshold level of 750 μg mL−1 in urine; hence, doping control laboratories have to establish quantitative and qualitative methods for its determination.
A simple and rapid liquid chromatographic/mass spectrometric method was developed and validated for the quantification and
identification of salicylic acid. Urine samples after 900-fold dilution and addition of the internal standard (4-methylsalicylic
acid) were directly injected to the liquid chromatography/quadrupole time-of-flight mass spectrometry system. Electrospray
ionization in negative mode with full scan acquisition mode and product ion scan mode were chosen for the quantification and
identification of salicylic acid, respectively. Run time was 2.0 min. The tested linear range was 2.5–50 μg mL−1 (after 100-fold sample dilution). The relative standard deviations of intra- and inter-assay analysis of salicylic acid in
horse urine were lower than 2.5% and 2.8%, respectively. Overall accuracy (relative percentage error) was less than 3.3%.
Method was applied to two real samples found to be positive for salicylic acid, demonstrating simplicity, accuracy, and selectivity. 相似文献
16.
Babu Rao Chandu Sreekanth Nama Kanchanamala Kanala Balasekhara Reddy Challa Rihana Parveen Shaik Mukkanti Khagga 《Analytical and bioanalytical chemistry》2010,398(3):1367-1374
A novel simple, sensitive, selective, and rapid high-performance liquid chromatography coupled with tandem mass spectrometry
method was developed and validated for quantification of riluzole in human plasma. The chromatography was performed by using
a Zorbax-SB-C18 (4.6 × 75 mm, 3.5 μm) column , isocratic mobile phase 0.1% formic acid/acetonitrile (10:90 v/v), and an isotope-labeled
internal standard (IS), [13C,15N2]riluzole. The extraction of drug and internal standard was performed by liquid–liquid extraction and analyzed by MS in the
multiple reaction monitoring (MRM) mode using the respective [M+H]+ ions, m/z 235.0/165.9 for riluzole and m/z 238.1/169.0 for the IS. The calibration curve was linear over the concentration range 0.5–500.0 ng/ml for riluzole in human
plasma. The limit of quantification (LOQ) was demonstrated at 0.5 ng/ml. The within-batch and between-batch precision were
0.6–2.3% and 1.4–5.7%, and accuracy was 97.1–101.1% and 98.8–101.2% for riluzole respectively. Drug and IS were eluted within
3.0 min. The validated method was successfully applied in a bioequivalence study of riluzole in human plasma. 相似文献
17.
A flow-cell for micro-porous membrane liquid–liquid extraction with a sheet membrane was used to extract 2-ethylhexyl 4-(dimethylamino)
benzoate (EDB) from urine of solar-cream users and spiked wine samples. The cell enabled the target analyte to be extracted
from 7.9 mL of donor solution into 200 μL of acceptor solution (decane). After extraction, the acceptor solution was transferred
to a micro-vial for GC-MS analysis without derivation. In this work, variables affecting the enrichment factor were also studied,
such as organic solvent, extraction time, recirculation flow of the donor solution through the donor chamber, presence of
potassium chloride and ethanol in the donor solution and pH. The method has been evaluated in terms of linearity, sensitivity,
precision, limits of detection and quantification and extraction efficiency. Limits of quantification were 1 and 3 μg L−1 EDB for urine and wine, respectively. Quantitative analysis has been carried out by applying the method of standard additions.
Within- and between-day relative standard deviations were lower than 12% and 20%, respectively. EDB was found in the urine
of users of cream containing EDB in the concentration interval 1.2–7.2 μg L−1. Therefore, this provides evidence of EDB dermal absorption and subsequent excretion through the urinary tract. EDB was not
found in the analysed wine samples. 相似文献
18.
Stankov-Jovanović VP Nikolić-Mandić SD Mandić LM Mitić VD 《Analytical and bioanalytical chemistry》2006,385(8):1462-1469
Pancuronium bromide (PCBr) inhibition effect on enzyme cholinesterase from pooled human serum (Che, EC 3.1.1.8 acylcholine
acylhydrolase) was used for development of a spectrophotometric kinetic method for PCBr determination in human serum and urine.
Optimal conditions for the basic and inhibitor reactions were established: pH=7.7 and substrate concentration c(benzoylcholine
chloride)=1.33 mmol/L. Kinetic parameters were also determined: Michaelis-Menten’s constant KM=0.40 mmol/L, maximal reaction rate Vmax=52.2 μmol/L min, inhibition constant Ki=0,56 μmol/L and IC50=1.31 μmol/L. Linear dependence between the reaction rate and inhibitor concentration exists in PCBr concentration range 8.20–68.25 nmol/L,
which corresponds to the real sample concentrations from 0.328 to 2.730 μmol/L. The method detection and quantification limits
were 2.01 nmol/L and 6.67 nmol/L, respectively. Precision of the method was tested for three pancuronium concentrations (10.70,
29.35 and 51.25 nmol/L). Relative standard deviation (RSD) was in the range 0.15–7.45%. Accuracy was examined by standard
addition method. Influence of the substances usually present in serum and urine on the reaction rate was tested. The developed
method was applied for PCBr content determination in serum model samples, urine model samples and in urine taken during surgery.
The method has good sensitivity, accuracy, precision and it is suitable for clinical practice.
相似文献
19.
Paula Guerra Ethel Eljarrat Damià Barceló 《Analytical and bioanalytical chemistry》2010,397(7):2817-2824
This paper describes the development of a methodology for the simultaneous determination and quantification of hexabromocyclododecane
(HBCD), tetrabromobisphenol A (TBBPA), and related compounds (bisphenol A, monobromobisphenol A, dibromobisphenol A, and tribromobisphenol
A) in sludge and sediment samples. The selected method is based on an extraction with dichloromethane: methanol followed by
purification via SPE C18 cartridges. Instrumental determination was carried out by liquid chromatography–quadrupole linear ion trap mass spectrometry
(LC-QqLIT-MS), with quantification based on isotopic dilution method. Analyte recoveries were in the range of 39–120% and
88–126% for spiked sewage and sediment, respectively. Repeatability of replicate extractions was better than 13% relative
standard deviation. Linearity was checked in the range of 0.05 and 25 injected nanograms. Limits of detection (LODs) and limits
of quantification (LOQs) were in the range of 0.6 and 2.7 ng/g and 1.4 and 66 ng/g for sediment and sludge samples, respectively.
The developed method was applied to sewage sludge and sediment samples collected along the Ebro River and Cinca River, one
of its tributaries (northeast of Spain). TBBPA levels in sewage sludge ranged from not quantified to 1,329 ng/g dw, whereas
levels in sediment samples were lower, between not detected and 15 ng/g dw. As regards HBCD, concentrations were between not
detected and 375 ng/g for sludge samples and 0.8 and 1850 ng/g for sediments. 相似文献
20.
Barrett B Borek-Dohalský V Fejt P Vaingátová S Huclová J Nemec B Jelínek I 《Analytical and bioanalytical chemistry》2005,383(2):210-217
A validated, highly sensitive, and selective HPLC method with MS–MS detection has been developed for quantitative determination
of azithromycin (AZI) in human Na2EDTA plasma. Roxithromycin (ROX) was used as internal standard. Human plasma containing AZI and internal standard was ultrafiltered
through Centrifree Micropartition devices and the concentration of AZI was determined by isocratic HPLC–MS–MS. Multiple reaction
monitoring mode (MRM) was used for MS–MS detection. The calibration plot was linear in the concentration range 2.55–551.43 ng mL−1. Inter-day and Intra-day precision and accuracy of the proposed method were characterized by R.S.D and percentage deviation,
respectively; both were less than 8%. Limit of quantification was 2.55 ng mL−1. The proposed method was used to determine the pharmacokinetic profile of AZI (250-mg tablets). 相似文献