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1.
Nitrosamines which have been detected in various latex products are carcinogens. The method for determination of volatile nitrosamines in latex products was developed using a combination of headspace solid phase micro-extraction (HS-SPME) and gas chromatography?Cmass spectrometry (GC?CMS). A carboxen/polydimethylsiloxane (CAR/PDMS) fiber was used for HS-SPME involving the following variables: (1) agitation conditions, (2) extraction temperature (3) extraction time, and (4) salt concentration. The instrument performances of three detection systems including GC combined thermal energy analyzer, nitrogen chemiluminescence detector and MS were evaluated. The agitation conditions including magnetic stirring and ultrasonication were investigated by the comparison of extraction efficiency of HS-SPME for nitrosamines. Obtained optimal detection conditions of nitrosamines were HS-SPME at 45 °C for 60 min assisted with magnetic stirring and saturated NaCl followed by GC?CMS. To evaluate this method performance, the commercial products including eleven latex products (gloves, balloons and condoms) and four liquid silicone nipples were analyzed with the method. The results revealed that the method is suitable for simple and effective determination of nitrosamines in latex products. The advantage of this HS-SPME?CGC?CMS method is simple treatment, fast analysis, adequate sensitivity and without organic solvent. 相似文献
2.
Xiujun Cao Guoxin Song Yihan Gao Jianfeng Zhao Minlu Zhang Weiping Wu Yaoming Hu 《Chromatographia》2009,70(3-4):661-664
A sensitive and rapid derivatization method for the simultaneous determination of chloropropanols [1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP) and 3-chloropropane-1,2-diol (3-MCPD)] has been developed. The three chloropropanols were silylated with 1-trimethylsilylimidazole and then determined by GC–MS. n-Undecane was used as the internal standard. The limits of detection (LOD) were 0.20, 0.10, 0.14 μg kg?1 for 1,3-DCP, 2,3-DCP and 3-MCPD, respectively. The three compounds behaved >0.999 of linearity and satisfactory precision with the relative standard deviation (RSD) <10%. The excellent validation data suggested that this method was more effective than heptafluorobutyrylimidazole derivatization, and 1-trimethylsilylimidazole was considered as a promising silylating reagent to be widely applied to measurements of chloropropanols in real samples. 相似文献
3.
Formaldehyde dimethylhydrazone (FADMH) is one of the important transformation products of residual rocket fuel 1,1-dimethylhydrazine (1,1-DMH). Thus, recent studies show that FADMH toxicity is comparable to that of undecomposed 1,1-DMH. In this study, a new method for quantification of FADMH in water based on solid phase microextraction (SPME) in combination with gas chromatography (GC) with mass spectrometric (MS) and nitrogen-phosphorus detection (NPD) is presented. Effects of SPME fiber coating type, extraction and desorption temperatures, extraction time, and pH on analyte recovery were studied. The optimized method used 65 micron polydimethylsiloxane/divinylbenzene fiber coating for 1?min headspace extractions at 30?°C. Preferred pH and desorption temperature from the SPME fiber are >8.5 and 200?°C, respectively. Detection limits were estimated to be 1.5 and 0.5?μg?L(-1) for MS and NPD, respectively. The method was applied to laboratory-scale experiments to quantify FADMH. Results indicate applicability for in situ sampling and analysis and possible first-time detection of free FADMH in water. 相似文献
4.
A rapid, sensitive and reliable LC?CMS?CMS method for the determination of eight benzimidazoles in animal feed was developed and validated. Samples were extracted with acidic acetonitrile. The extract was diluted with 0.1% formic acid in water, and analyzed by LC?CMS?CMS on a Waters XBridge? C18 column with acetonitrile/0.1% formic acid in water as mobile phase. The samples were quantified with the matrix standard calibration curve method. Good linearity was obtained for eight benzimidazoles at a concentration of 0.005?C2.5 ??g mL?1 with a linear relative coefficient more than 0.990. Recoveries of 84.0?C104.0% with CVs of 2.50?C7.50% were obtained. Limit of detection was 2.1?C63.0 ??g kg?1. The method demonstrated to be suitable for the determination of eight benzimidazoles in animal feed samples. 相似文献
5.
Adam Clarke James P. Scarth Jonathan Hands Philip Teale Aileen C. Mill Roy Macarthur Jack Kay 《Chromatographia》2011,73(11-12):1155-1169
Under European legislation, the use of anabolic steroids as growth promoters in meat production is prohibited. Currently, there is no internationally accepted method used for the detection of the potentially endogenous steroids nandrolone and boldenone in the ovine. In the current study, a multi-residue GC?CMS?CMS-based urinary assay has been validated for boldenone as well as the nandrolone metabolites 5??-estrane-3??,17??-diol and epinandrolone. Using a standard addition calibration line approach in pooled bovine urine, the method was linear between the endogenous concentrations and those augmented with 6,000 pg mL?1. The method was then applied to populations of wether (n = 242) and ewe (n = 237) ovine animals in order to establish urinary thresholds for detecting nandrolone and boldenone abuse. A statistical model (the Chebyshev inequality) was used to produce threshold concentrations for each analyte. Adjustment of the nandrolone metabolite data for specific gravity, a measure of the hydration status of the animal, allowed the effective thresholds to be reduced; potentially leading to a lower number of false positives. Furthermore, the proposed epinandrolone confirmatory thresholds (38,628 and 57,950 pg mL?1 in wethers and ewes, respectively) were found to be effective in detecting abuse of nandrolone for at least 1 month post-dose of this steroid. However, further studies would be required to assess the efficacy of the proposed boldenone confirmatory thresholds (19,857 and 56,080 pg mL?1 in wethers and ewes, respectively) since data on its excretion following administration to the ovine are lacking. 相似文献
6.
Qi Yu Zhe-Yi Hu Fan-Yuan Zhu Jin-Hui Zhu Li-Li Wan Yan Li Cheng Guo 《Chromatographia》2011,73(3-4):257-262
Combination drug products containing amlodipine and atorvastatin are widely marketed and used in the treatment of concomitant hypertension and dyslipidemia. A rapid, simple and sensitive high performance liquid chromatography?Ctandem mass spectrometry (HPLC?CMS?CMS) method for determination of atorvastatin and amlodipine in plasma of hypertensive patients has been developed and validated to be used for therapeutic drug monitoring. The plasma samples were subjected to methanol protein precipitation. Chromatographic separation was performed on a C18 column using a gradient elution. The mobile phase consisted of 0.1% of formic acid in water and 0.1% of formic acid in acetonitrile and was pumped at a flow rate of 0.4 mL min?1. Detection of analytes was achieved by tandem mass spectrometry with electrospray ionization (ESI) interface in positive ion mode. The calibration curves were linear over the range of 0.46?C1,000 ng mL?1. The intra- and inter-day precisions were within 12.2%, while the accuracy ranged from 92.7 to 108.1%. The validated LC?CMS?CMS method was successfully applied for the determination of atorvastatin and amlodipine in plasma of hypertensive patients. 相似文献
7.
Ultrasound-assisted dispersive liquid?Cliquid microextraction (USA-DLLME) with low solvent consumption was demonstrated for gas chromatography-mass spectrometry (GC?CMS) determination of 16 typical polycyclic aromatic hydrocarbons (PAHs) in seawater samples. Factors affecting the extraction process, such as extraction and dispersive solvent, phase ratio, temperature, extraction and centrifugation time, were investigated thoroughly and optimized. The linear range was 20?C2,000 ng L?1 except for acenaphthylene (Acy) at 10?C2,000 ng L?1 and phenanthrene (Phe), fluoranthene (Flu) and pyrene (Py) all at 5?C2,000 ng L?1. Enrichment factors (EFs) ranging from 722 to 8,133 were obtained, achieving limits of detection at 1.0?C10.0 ng L?1. The method attained good precision (relative standard deviation, RSD) from 3.4 to 14.2% for spiked 50 ng L?1 individual PAHs standards. Method recoveries were in the range 87?C124% and 70?C127% for spiked samples from simulated seawater and beach seawater, respectively. The proposed USA-DLLME helped to obtain about 1.1?C10 times higher EFs in a minimum amount of solvent and in less time than traditional DLLME. 相似文献
8.
Haoyan Xu Tianyi Wang Qi Zhao Qinglei Zeng Hui Wang Yang Xu Xiaopan Zhang Feng Wang Lan Ding 《Chromatographia》2011,74(3-4):267-274
An environmentally friendly method for the determination of fluoroquinolone (FQ) antibiotics including enrofloxacin, ciprofloxacin, levofloxacin, fleroxacin and sparfloxacin in four feeds is proposed. Disodium ethylenediaminetetraacetate (EDTA)?CMcllvaine buffer (0.1 mol L?1, pH 4.0) was used as an extracting solvent and the extraction process was accelerated by microwave irradiation. No organic solvents were used in the extraction procedure. The extract obtained was then cleaned up and concentrated by an Oasis hydrophilic?Clipophilic balance (HLB) solid-phase extraction cartridge. The relative intra- and inter-day standard deviations obtained were in the range of 3.7?C9.1 and 2.1?C11.4%, respectively. In the three fortified levels of blank feed sample (30, 100 and 500 ng g?1), recoveries of FQs ranging from 61.1 to 97.9% were obtained. The analytes desorbed from HLB were analyzed by liquid chromatography?Ctandem mass spectrometry. The limit of detection was in the range of 5.0?C9.1 ng g?1. The method presented here can be considered a promising alternative to traditional techniques using shaking or stirring for extraction, being more effective, and producing less pollution. 相似文献
9.
Changyuan Wang Jian Cang Qi Liu Qiang Meng Huijun Sun Ying Gao Decheng Lv Taiichi Kaku Kexin Liu 《Chromatographia》2011,73(5-6):481-486
A rapid and selective liquid chromatographic/tandem mass spectrometric method for the determination of JBP485 was developed and validated. Following protein precipitation, the analyte and internal standard (JBP923) were separated from human plasma using an isocratic mobile phase on an Elite Kromasil C18 column. An API 3200 tandem mass spectrometer equipped with a Turbo ionSpray ionization source was used as the detector and operated in the positive ion mode. Multiple reaction monitoring using the precursor to product ion combinations of m/z 201.2 ?? 86.2 and m/z 219.2 ?? 86.2 was performed to quantify JBP485 and JBP923, respectively. The method was linear in the concentration range of 0.10?C50.00 ??g mL?1 using 100 ??L of plasma. The lower limit of quantification was 0.10 ??g mL?1. The intra- and inter-day relative standard deviations over the entire concentration range were less than 6.65%. Accuracy determined at three concentrations (0.25, 4.00 and 25.00 ??g mL?1 for JBP485) ranged from ?0.78 to 2.74% in terms of relative error. Each plasma sample was chromatographed within 2.0 min. The method was successfully applied to characterize the pharmacokinetic profiles of JBP485 in rats after an intravenous injection of 6.25 mg kg?1 JBP485. 相似文献
10.
Guang-Tao Hao Yan Chen Rui-Hua Dong Heng-Yan Qu Yu-Guang Liang Yuan-Yuan Li Zhuan-Jie Zheng Hong-Zhi Gao Ze-Yuan Liu 《Chromatographia》2011,74(7-8):567-574
A rapid, sensitive and specific assay method has been developed to simultaneously determine human plasma concentrations of hydrocodone and its metabolites, norhydrocodone, hydromorphone, using high-performance liquid chromatography with an electrospray ionization (ESI) tandem mass spectrometry (HPLC?CMS?CMS). Hydrocodone, its metabolites, and internal standard, hydrocodone-d 3, norhydrocodone-d 3, hydromorphone-d 3, were separated from human plasma using solid-phase extraction (Empore MPC-SD Solid Phase Extraction Disk). The eluate was dried, reconstituted and injected into the LC?CMS?CMS system. Chromatographic separation was performed on a Kromasil 100-5SIL-Dimensions C18 column (100 × 2.1 mm, 5.0 ??m, Thermo Hypersil-Keystone, USA) using a gradient mobile phase with 20 mmol L?1 ammonium formate in water with 0.2% formic acid and 0.1% formic acid in acetonitrile. Detection and quantitation were performed by MS/MS using electrospray ionization and multiple reactions monitoring in the positive ion mode. The calibration curves were linear over the concentration ranges 0.05?C50 ng mL?1 for hydrocodone (r 2 = 0.9991) and norhydrocodone (r 2 = 0.9990), and 0.01?C10 ng mL?1 for hydromorphone (r 2 = 0.9990). The limit of quantification was 0.05 ng mL?1 for hydrocodone and norhydrocodone, and 0.01 ng mL?1 for hydromorphone. The extraction recovery was above 64.36, 68.51 and 71.78% for hydrocodone, norhydrocodone and hydromorphone. The accuracy was higher than 99.06, 97.70 and 100.07% for hydrocodone, norhydrocodone and hydromorphone. The intra- and inter-day precisions were <5.80, 5.90 and 3.02% for hydrocodone, norhydrocodone and hydromorphone. The method was accurate, sensitive and simple and was successfully applied to a pharmacokinetic study after a single oral administration of hydrocodone bitartrate at a dose of 5 mg in 12 healthy Chinese volunteers. 相似文献
11.
Zhongyang Liu Guangzhi Gu Huimin Xia Qiang Liu Zhiqing Pang Xinguo Jiang Jun Chen 《Chromatographia》2011,74(3-4):227-234
A reversed-phase liquid chromatography coupled to tandem mass spectrometry (LC?CMS?CMS) method was developed and validated for the determination of fulvestrant in rat plasma. Sample preparation involved a liquid-liquid extraction using 1.0 mL of n-hexane?Cisopropanol (90:10, v/v) to extract the analyte from 0.1 mL of rat plasma. The analytes were separated on a phenyl-based column using the mobile phase consisting of methanol/water containing 5 mM ammonium acetate at the flow rate of 0.3 mL min?1. The analytes were monitored by tandem mass spectrometry under electrospray negative ionization mode. Linear calibration curves were generated over the fulvestrant concentration ranges of 0.05?C10.0 ng mL?1 in rat plasma. The accuracy and within- and between-day precisions were within the generally accepted criteria for bioanalytical methods (<15%). This developed and validated assay method was successfully employed to characterize the plasma concentration-time profile of fulvestrant after its intramuscular administration in rats at a dose of 10 mg kg?1. 相似文献
12.
Peng Yu Guoping Yang Hongyi Tan Zeneng Cheng Ming Song Zhenkun Gu Xiao Li 《Chromatographia》2011,73(9-10):921-927
A sensitive, specific and rapid high performance liquid chromatography?Catmospheric pressure chemical ionization source-tandem mass spectrometry (LC-APCI-MS-MS) method for the determination of pilocarpine in human plasma was developed and validated. The method is based on liquid?Cliquid extraction, followed by a reversed-phase liquid chromatographic separation, and detected by means of tandem mass spectrometry. The linear calibration curve covered a concentration range of 2?C500 ??g L?1. The intra- and inter-day precisions for pilocarpine were <10% and the accuracies were between 90 and 110%. The method was applied successfully to a pharmacokinetic study involving 20 healthy Chinese male volunteers after oral administration of 6 mg pilocarpine. 相似文献
13.
Hubert P. O. Tang Shirley S. L. Lai Ashley Y. H. Lai W. O. Lee 《Chromatographia》2009,70(9-10):1405-1410
A specific and sensitive analytical method for the quantitative determination of cyanuric acid in animal feed was developed. Sample preparation involved the diethylamine/acetonitrile/water extraction of feed using sonication and shaking. The extract was subjected to clean-up by dual solid phase extraction using mixed mode anionic and cationic extraction cartridges. After removal of clean-up solvent, cyanuric acid was converted to a tert-butyldimethylsilyl derivative and was determined by gas chromatography–mass spectrometry in the selected ion monitoring mode. 13C 3 15 N3-cyanuric acid was employed as the internal standard. The calibration curve was found to be linear up to 4 mg kg?1. LOD and LOQ were determined to be 0.06 to 0.4 mg kg?1 for fish and chicken feed. The mean recovery of cyanuric acid was 96 to 98% with relative pooled standard deviation of 1.8–7.4% in the range of 0.5 to 100 mg kg?1 for fish and chicken feed. The validated method was applicable for analysing cyanuric acid in animal feed. 相似文献
14.
Determination of Imidol in Rat Plasma by UPLC�CMS�CMS and Its Application in a Pharmacokinetic Study
Zhong-Bo Liu Qing Li Wei Li Xiao-Wei Song Guang-Ping Rong Yan-Fang Zhao Ping Gong Kai-Shun Bi Xiao-Hui Chen 《Chromatographia》2011,74(1-2):59-66
A rapid, sensitive and accurate ultra-performance liquid chromatography/tandem mass spectrometry method was developed and validated for the quantitative determination of imidol in rat plasma for the first time. The analyte and internal standard were extracted from plasma by liquid?Cliquid extraction with diethyl ether. The separation was performed on a BEH C18 column (50 mm × 2.1 mm, 1.7 ??m). The detection was carried out by electrospray ionization mass spectrometry in positive ion mode with multiple reaction monitoring. Linear calibration curves were obtained in the concentration range of 2.5?C2,500 ng mL?1, with the lower limit of quantification of 2.5 ng mL?1. The intra- and inter-day precision (RSD) values were below 8% and accuracy (RE) was from ?7.9 to 6.3%. After strict validation, the method was applied successfully to the pharmacokinetic study of imidol in rats after oral and intravenous administration, respectively. 相似文献
15.
Sarcosine, an isomer of l-alanine, has been recently proposed as a potential biomarker for prostate cancer risk and aggressiveness, while some studies debated its importance. As both sarcosine and l-alanine are present in human urine, it is a great challenge to separate and accurately quantify these isobaric (i.e., same m/z) compounds by chromatographic separation and mass spectrometric detection. In this study, we developed a novel 1,3-dipolar cycloaddition derivatization method that resolves sarcosine from l-alanine and allows accurate quantification of sarcosine in human urine by gas chromatography–mass spectrometry (GC–MS). This novel derivatization approach was specific to sarcosine only, while the common silylanization method resulted in overlapped derivates of both sarcosine and l-alanine. The derivatization conditions, including reagent amount, reaction temperature and time, were optimized. The method developed here has excellent precision (relative standard deviation <4.7 %, n = 5), good linearity (slope = 0.2408; r 2 = 0.9996, 0.1–100 μg mL?1), and a low limit of detection in human urine (0.15 ng mL?1). Application of this analytical method to urine samples spiked with standard sarcosine indicates that it is a robust and powerful alternative for resolving and quantifying sarcosine from l-alanine isomer in human urine by GC–MS. 相似文献
16.
A simple, rapid and sensitive hollow-fiber with drop-to-drop solvent microextraction (HF-DDSME) combined with gas chromatography?Cmass spectrometry (GC?CMS) has been successfully developed for extraction and determination of antidepressants drugs (AD) in blood sample. The parameters that affect the separation and preconcentration of AD from sample solution were investigated. Calibration curve obtained for three AD were in the range of 100?C1,000; 150?C1,200; and 80?C1,200 ng mL?1 for amitriptyline, imipramine, and promethazine, respectively, with correlation coefficient (R 2 ) between 0.990 and 0.997. The limit of detection (LOD) obtained for amitriptyline, imipramine and promethazine was 25, 30 and 18 ng mL?1, respectively. The developed method has been successfully applied for the determination of AD concentration in blood sample, and the recoveries for the spiked samples were in the range of 92.3?C97.6%. The sample preparation procedure is very simple, effective and virtually solvent-free, and indicated to be a good alternative for the traditional liquid?Cliquid extraction. Finally, the proposed method was successfully applied for the determination of drug concentration of AD in human blood sample. 相似文献
17.
Xin Zheng Pei Hu Jian Liu Qian Zhao Mengzhao Wang Ji Jiang Wei Zhong 《Chromatographia》2011,74(1-2):41-49
A specific, sensitive, and rapid method based on high-performance liquid chromatography coupled to tandem mass spectrometry (LC?CMS?CMS) was developed for determination of gefitinib in human serum and cerebrospinal fluid (CSF). The analyte was detected by tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring (MRM). Gefitinib was extracted from serum or CSF samples with ethyl acetate using icotinib as internal standard. The method was validated over the concentration range of 1.00?C1,000 ng mL?1 in human serum and 0.05?C50.0 ng mL?1 in CSF. For both matrices, inter- and intraday precision (CV%) were less than 15% and accuracy was within 85?C115%. Average extraction recoveries were 78.9 and 61.8% in human serum and CSF, respectively. Linearity, recovery, matrix effects, and stability were validated in the two matrices. The method was successfully used for analysis of clinical samples from lung cancer patients with brain metastases treated with gefitinib in the dosage range of 250?C500 mg day?1. 相似文献
18.
Liberato Brum Junior Manoela Guerra Leal Fl��via de Toni Uchoa Moacir Kaiser S��lvia Stani?uaski Guterres Teresa Dalla Costa 《Chromatographia》2011,73(11-12):1081-1088
A fast, sensitive, and specific LC?CMS?CMS method for determination of quinine (QN) and doxycycline (DOX) in rat plasma has been developed and validated. QN, DOX, and cimetidine (internal standard, IS) were extracted from the plasma by protein precipitation. The compounds were separated on a C18 column with methanol?C0.1% aqueous formic acid 70:30 (v/v) as mobile phase at a flow rate of 0.5 mL min?1 (split 1:3). Detection was by positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, monitoring the transitions 325.0 ?? 307.0, 445.0 ?? 428.1, and 252.8 ?? 159.0, for QN, DOX, and IS, respectively. The analysis was carried out in 2.0 min and the method was linear in the plasma concentration range 5?C5,000 ng mL?1. The mean extraction recoveries for QN, DOX, and IS from plasma were 89.4, 90.5, and 86.3%, respectively. The method was validated for linearity, precision, accuracy, specificity, and stability; the results obtained were within the acceptable range. The proposed method was successfully applied to the determination of QN and DOX in rat plasma samples to support pharmacokinetic studies. 相似文献
19.
A new facile, rapid, inexpensive, and sensitive method based on magnetic micro-solid phase extraction (M-??-SPE) coupled to gas chromatography?Cmass spectrometry (GC?CMS) was developed for determination of the herbicide oxadiargyl in environmental water samples. The feasibility of employing non-modified magnetic nanoparticles (MNPs) as sorbent was examined and applied to perform the extraction process. Influential parameters affecting the extraction efficiency along with desorption conditions were investigated and optimized. The limit of detection (LOD, S/N = 3) and limit of quantification (LOQ, S/N = 10) of the method under optimized conditions were 0.005 and 0.030 ng mL?1, respectively. The relative standard deviations (RSD) (n = 3) at a concentration of 0.10 ng mL?1 was 11%. The calibration curve of oxadiargyl showed linearity in the range of 0.050?C0.50 ng mL?1. The developed method was successfully applied to the extraction of oxadiargyl from spiked tap water and Zayande-Rood River water samples and the relative recoveries of 98 and 94% were obtained, respectively. 相似文献
20.
A fast and effective sample cleanup procedure for the quantification of polycyclic aromatic hydrocarbons (PAHs) in fish samples is presented. The procedure involved extraction of fish samples using acetonitrile and cleanup by an automated gel-permeation chromatography (GPC) following liquid?Cliquid partition into n-hexane. The extracted samples were analyzed by gas chromatography-mass spectrometry (GC?CMS). Electron ionization was employed in a single analysis for the determination of PAHs in the selected ion monitoring mode. Three different solvents were studied for the extraction step: acetonitrile/n-hexane, methanol/n-hexane and acetone/n-hexane. The best solvent was found to be acetonitrile/n-hexane. The cleanup technique resulted in a good separation of analytes from co-extractive matrix compounds. 相似文献