To develop a simple and rapid method for the simultaneous determination of nicotine and its nine metabolites in rat blood, an in vivo microdialysis sampling technique coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for quantitation and characterization of the pharmacokinetics of nicotine and its metabolites. Microdialysis probes were inserted into the jugular vein of Sprague Dawley rats, and dialysates were collected after nicotine (0.5 mg/kg, i.p.) administration. Target analytes and corresponding deuterated internal standards were separated on a hydrophilic interaction liquid chromatography column (HILIC BEH 2.1. × 150 mm, 1.7 μm) and detected by UPLC-MS/MS under multiple reaction monitoring mode. The limits of quantification for nicotine and its nine metabolites ranged from 0.039 to 0.46 ng/mL. Intra- and inter-day precision and accuracy were well within the predefined limits of acceptability (<11 %). Pharmacokinetic results showed that the mean half-lives of nicotine, cotinine, nornicotine, norcotinine, nicotine-N'-oxide, cotinine-N'-oxide, trans-3'-hydroxy-cotinine, nicotine-N-glucuronide, cotinine-N-glucuronide, and trans-3'-hydroxy-cotinine-O-glucuronide in rat plasma were 63, 291, 175, 440, 251, 451, 322, 341, 488, and 516 min, respectively. The blood concentration-time profiles of nicotine and its nine metabolites indicate that nicotine is rapidly consumed after the administration and subsequently cotinine is generated as the main metabolite; meanwhile, cotinine and other eight minor metabolites exhibit longer retention times in rat body.
Tobacco-specific N-nitrosamines (TSNAs), including N'-nitrosonornicotine, 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone, N'-nitrosoanatabine, and N'-nitrosoanabasine, have been implicated as a source of carcinogenicity in tobacco and cigarette smoke. We present a rapid and effective method comprising SPE based on tetraazacalix[2]arene[2]triazine-modified silica as sorbent and analysis with HPLC-MS/MS for the determination of TSNAs and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL), a metabolite of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone, in rabbit plasma. The linear dynamic ranges were 10-2000 pg/mL for NNAL and 4-2000 pg/mL for the four TSNAs with good correlation coefficients (>0.9965). The LODs were in the range of 0.9-3.7 pg/mL, and the LOQs were between 2.9 and 12.3 pg/mL. The accuracies of the method were also evaluated and found to be in the range of 90.1-113.3%. This method is promising to be applied to the preconcentration and determination of TSNAs and NNAL in smoke and human body fluids.
The examined issue of tissue vibration due to the operation power device is a significant problem. The proposed method can be used by a surgery robot, and then spinal surgery may greatly benefit from the enhanced safety of robotics.
Once in the hands of end users, such durable equipment as spacecraft, aircraft, ships, automobiles, computers, etc. are in a state of debugging, working or storage. In either state, availability, reliability and super-efficiency are the ultimate goals, which have been achieved through constant monitoring as well as regular, preventive, routine and corrective maintenance. Although some advanced instruments can visualize certain invisible malfunctioning phenomena into visible ones, deeply hidden troubles cannot be found unless monitoring and testing data are addressed using tools that process the data statistically, analytically and mathematically. Some state-of-theart trouble-shooting and life-predicting techniques and approaches are introduced in this paper. ª 2015 Production and hosting by Elsevier Ltd. on behalf of CSAA & BUAA.
BackgroundIn anterior cervical discectomy and fusion (ACDF) surgery, drilling operation causes a high risk of tissue injury. This study aimed to present a novel feedback system based on sound pressure signals to identify drilling condition during ACDF.Material/MethodsACDF surgery was performed on the C4/5 segments of 6 porcine cervical specimens. The annulus fibrosus, endplate cartilage, sub-endplate cortical bone, and posterior longitudinal ligament (PLL) were drilled until penetration using a 2-mm high-speed burr. Sound pressure signals were collected using a microphone and dynamic signal analyzer. The recorded signals of different tissues were proceeded with lifting wavelet transform for extracting harmonic components. The frequencies of harmonic components are 1, 2, 3, 4, and 5 times higher than the motor frequency. The magnitude of harmonic components was calculated to identify different drilling conditions, along a broad spectrum of frequencies (1–5 kHz). For statistical analysis, one-way ANOVA (analysis of variance) and post hoc test (Dunnett’s T3) were performed.ResultsVery good demarcation was found among the signal magnitudes of different drilling conditions. Different drilling conditions do not present the same rate of variation of frequency. Differences in magnitude among all drilling conditions were statistically significant at certain frequency points (p<0.05). In 3 cases, one tissue could not be identified with respect to another (annulus fibrosus and endplate cartilage at 2 kHz, PLL and penetration at 3 kHz, annulus fibrosus and sub-endplate cortical bone at 5 kHz, p>0.05).ConclusionsSound pressure signals may provide an auxiliary feedback system for enhancing drilling operation in ACDF surgery, especially in minimally invasive surgery.
In this paper, we propose a new strategy for separation and determination of tobacco-specific N-nitrosamines (TSNAs), a group of strong carcinogens found only in tobacco products, by using CZE and CE-MS associated with SPE. Six TSNAs: N'-nitrosonornicotine, N'-nitrosoanatabine, N'-nitrosoanabasine, 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone, 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol, and 4-(methylnitrosamino)-4-(3-pyridyl)-1-butanol were simultaneously separated by either of two CZE methods, one of which worked with ammonium formate buffer (pH 2.5) and another with citrate buffer (pH 2.4), as well as a CE-MS method. The CZE conditions including pH and concentration of running buffer, capillary length, applied voltage, and capillary temperature were systematically optimized. For CE-MS method, an optimized sheath liquid consisted of methanol-water was used at a flow rate of 10 muL/min. With SPE procedure, our proposed CE-MS method was successfully applied to determine TSNAs after 15 min metabolism in rabbits. A comparison study between CZE and CE-MS methods for quantitative purposes was carried out, showing that both methods provided similar separation efficiency, selectivity, repeatability, linearity, and recovery. However, CE-MS method was better suited for the analysis of TSNAs in complicated biological samples for its sensitivity and extra information on molecular structure. Having good accordance with our previous work by using LC-MS, the new CE-MS method is expected to be an alternative to the LC-MS method and applied to study the metabolism of TSNAs.
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