Dispersive liquid–liquid microextraction of quinolones in porcine blood: Validation of a CE method using univariate calibration or multivariate curve resolution‐alternating least squares for overlapped peaks

In the previously published part of this study, we detailed a novel strategy based on dispersive liquid–liquid microextraction to extract and preconcentrate nine fluoroquinolones in porcine blood. Moreover, we presented the optimized experimental conditions to obtain complete CE separation between target analytes. Consequently, this second part reports the validation of the developed method to determine flumenique, difloxacin, enrofloxacin, marbofloxacin, ofloxacin, ciprofloxacin, through univariate calibration, and enoxacin, danofloxacin, and gatifloxacin through multivariate curve resolution analysis. The validation was performed according to FDA guidelines for bioanalytical assay procedures and the European Directive 2002/657 to demonstrate that the results are reliable. The method was applied for the determination of fluoroquinolones in real samples. Results indicated a high selectivity and excellent precision characteristics, with RSD less than 11.9% in the concentrations, in intra‐ and interassay precision studies. Linearity was proved for a range from 4.00 to 30.00 mg/L and the recovery has been investigated at four different fortification levels, from 89 to 113%. Several approaches found in the literature were used to determinate the LODs and LOQs. Though all strategies used were appropriate, we obtained different values when using different methods. Estimating the S/N ratio with the mean noise level in the migration time of each fluoroquinolones turned out as the best studied method for evaluating the LODs and LOQs, and the values were in a range of 1.55 to 4.55 mg/L and 5.17 to 9.62 mg/L, respectively.     

Chemometrics‐assisted chromatographic fingerprinting: An illicit methamphetamine case study

The volatile chemical constituents in complex mixtures can be analyzed using gas chromatography with mass spectrometry. This analysis allows the tentative identification of diverse impurities of an illicit methamphetamine sample. The acquired two‐dimensional data of liquid–liquid extraction was resolved by multivariate curve resolution alternating curve resolution to elucidate the embedded peaks effectively. This is the first report on the application of a curve resolution approach for chromatogram fingerprinting to identify particularly the embedded impurities of a drug of abuse. Indeed, the strong and broad peak of methamphetamine makes identifying the underlying peaks problematic and even impossible. Mathematical separation instead of conventional chromatographic approaches was performed in a way that trace components embedded in methamphetamine peak were successfully resolved. Comprehensive analysis of the chromatogram, using multivariate curve resolution, resulted in elution profiles and mass spectra for each pure compound. Impurities such as benzaldehyde, benzyl alcohol, benzene, propenyl methyl ketone, benzyl methyl ketone, amphetamine, N‐benzyl‐2‐methylaziridine, phenethylamine, N ,N ,α‐trimethylamine, phenethylamine, N ,α,α‐trimethylmethamphetamine, N‐acetylmethamphetamine, N‐formylmethamphetamine, and other chemicals were identified. A route‐specific impurity, N‐benzyl‐2‐methylaziridine, indicating a synthesis route based on ephedrine/pseudoephedrine was identified. Moreover, this is the first report on the detection of impurities such as phenethylamine, N ,α,α‐trimethylamine (a structurally related impurity), and clonitazene (as an adulterant) in an illicit methamphetamine sample.     

On Cartan's theorem for linear operators

In this paper, we describe a second main theorem of holomorphic curves in , of hyper‐order strictly less than 1, that involves a general linear operator . As an application, we derive a truncated second main theorem of degenerate holomorphic curves of hyper‐order strictly less than 1 using Nochka weights.     

Pseudo‐spherical normal Darboux images of curves on a lightlike surface

We introduce the notions of the pseudospherical normal Darboux images for the curve on a lightlike surface in Minkowski 3‐space and study these Darboux images by using technics of the singularity theory. Furthermore, we give a relation between these Darboux images and Darboux frame from the viewpoint of Legendrian dualities.     

Evolution of highly symmetric curves under the shrinking curvature flow

Under the shrinking curvature flow with inner normal velocity V = k^α(α > 1), it is shown that highly symmetric, locally convex initial curves evolve into a point asymptotically like an multi‐circles. The proof relies on a crucial use of Bonnensen inequality for highly symmetric, locally convex curves. Copyright © 2016 John Wiley & Sons, Ltd.     

超声弹性成像参数联合血清MK和VEGF对分化型甲状腺癌的诊断价值及与肿瘤恶性程度关系研究

本研究选取了分化型甲状腺癌(DTC)患者106例为甲状腺癌组,同期106例甲状腺腺瘤患者为甲状腺腺瘤组,检测比较了两组患者的超声弹性成像参数(弹性比值、蓝色面积比值)、血清中期因子(midkine,MK)、血管内皮生长因子(VEGF)水平。研究结果发现,弹性比值、蓝色面积比值、血清MK和VEGF水平与DTC患者淋巴结转移、包膜侵犯、临床分期相关(P<0.05);弹性比值、蓝色面积比值、血清MK和VEGF水平联合诊断DTC的曲线下面积(AUC)为0.888;弹性比值、蓝色面积比值、血清MK及VEGF水平与DTC患者组织中趋化因子受体(CXCR)4、解聚素金属蛋白酶(ADAM)9、靶向Xklp2靶蛋白(TPX2)基因表达量呈正相关,与程序性细胞死亡因子(PDCD)4基因表达量呈负相关。这些结果提示超声弹性成像参数、血清MK及VEGF水平上调可能用来评估DTC患者病情程度及肿瘤恶性程度,三者联合对DTC具有可靠诊断价值,可为临床诊治提供参考。     

螺旋CT成像联合血清copeptin、IL-18水平检测在急性脑梗死患者神经功能及预后评估中的应用价值

本文选取74例急性脑梗死(ACI)患者作为研究对象,入院时根据美国国立卫生院卒中量表(NIHSS)评分分为重度组(NIHSS评分>15分,n=21)、中度组(NIHSS评分5~15分,n=24)、轻度组(NIHSS评分<5分,n=29),均接受血清copeptin和IL-18水平检测及螺旋CT成像检查。结果发现,随ACI神经功能缺损加重,血清copeptin、白细胞介素18(IL-18)水平及峰值时间升高,CBV、CBF异常下降。经ROC曲线显示,血清IL-18联合CBF预测ACI患者预后不良的曲线下面积(AUC)最大。由上述结果可见螺旋CT成像参数、血清copeptin、IL-18水平与ACI患者神经功能存在一定相关性,三者联合为临床实现ACI患者个体化治疗和改善预后提供了可能。