Isolation, structure elucidation, and high-performance liquid chromatography quantification of photolytic degradation impurities in acrivastine.

Acrivastine is a second-generation H1-receptor antagonist, and its structure is sensitive to ultraviolet. Four unknown and one reported degradation products can be detected in the ultraviolet radiation solutions of acrivastine. To improve the quality control of acrivastine, the photodegradation impurities were isolated and structurally elucidated. There are four new impurities (1-3 and 5), and one reported compound (4). The isolation strategy was designed as preparative high-performance liquid chromatography using a reversed phase column with volatile acid addition in the mobile phase, combined with preparative thin-layer chromatography using silica gel with alkaline addition in the mobile phase. Using the developed methods, five impurities (1-5) were efficiently purified after two or three chromatography runs with purities > 95%. The structures of compounds 1-5 are elucidated based on spectroscopy analysis of MS, and nuclear magnetic resonance spectroscopy. Using the impurity standard, the high-performance liquid chromatography method was developed and validated. The method was proved to be sensitive, accurate (Recovery% 96.1-107.7%), linear (0.15-0.75 µg/mL, R2 > 0.996), robust, and specific, and it was successfully used to determine the degradation impurities of acrivastine and its formulation.

[Study on the Relationship between Soil Emissivity Spectra and Content of Soil Elements].

In this paper, based on the measurements of soil elements content and infrared spectra of 26 soil samples collected in more than 10 places, the relationship between soil emissivity in mid-infrared bands and the content of 11 soil elements including organic matters such as NO(3)-N, P, K, Ca, Mg, Cu, Fe, Mn, Zn and pH are analyzed. The bands where the soil elements content are significantly correlated with emissivity are given. And soil elements content estimation method is established based on the soil emissivity spectra with the partial least squares regression model and multiple stepwise regression model. The results show that: (1) In 8~10 µm, the correlation coefficient (R(2)) between Ca and soil emissivity is the highest, followed by Mg, Mn and Fe, with the highest correlation coefficient of 0.85 and the lowest, 0.52. In the range of 6~8 µm, the correlations between the contents of K, Fe, NO(3)-N, Zn and emissivity decrease gradually, with the highest correlation coefficient of 0.75 and the lowest 0.48. In 10~14 µm, the correlation between soil elements contents and emissivity is the highest for Mn, followed successively by P and K. (2) The scatter plot of soil emissivity and pH value has a parabola relation basically. The emissivity is the highest when pH value is 7, while the emissivity decreases gradually with the gradual decrease of pH value. (3) The accuracy of the estimated soil elements content from the partial least squares regression method is higher than that from the multiple stepwise regression method. It is noted that R(2) between the measurements and the estimates for the elements of Cu, Fe and Ca from the partial least squares regression method are very high (larger than 0.9). Additionally, using the simulated emissivity spectrum in the ASTER thermal infrared bands, modeling R(2) and validation R(2) between the measurements and the estimates for the elements of Ca from the multiple stepwise regression method are high (0.774 and 0.892, respectively). Using the simulated emissivity spectrum in the MODIS infrared bands, modeling R(2) and validation R(2) for Ca and Fe are higher than 0.85, and modeling R(2) and validation R(2) for Mg, K are higher than 0.5. As a whole, the emissivity spectrum in ASTER band 10 and band 11 and MODIS bands 28, 29, 30 are more sensitive to soil elements content, and thus they are more suitable for the estimation of soil elements content.

[An optical-fiber-sensor-based spectrophotometer for soil non-metallic nutrient determination].

In order to achieve rapid, convenient and efficient soil nutrient determination in soil testing and fertilizer recommendation, a portable optical-fiber-sensor-based spectrophotometer including immersed fiber sensor, flat field holographic concave grating, and diode array detector was developed for soil non-metallic nutrient determination. According to national standard of ultraviolet and visible spectrophotometer with JJG 178-2007, the wavelength accuracy and repeatability, baseline stability, transmittance accuracy and repeatability measured by the prototype instrument were satisfied with the national standard of III level; minimum spectral bandwidth, noise and excursion, and stray light were satisfied with the national standard of IV level. Significant linear relationships with slope of closing to 1 were found between the soil available nutrient contents including soil nitrate nitrogen, ammonia nitrogen, available phosphorus, available sulfur, available boron, and organic matter measured by the prototype instrument compared with that measured by two commercial single-beam-based and dual-beam-based spectrophotometers. No significant differences were revealed from the above comparison data. Therefore, the optical-fiber-sensor-based spectrophotometer can be used for rapid soil non-metallic nutrient determination with a high accuracy.

[Determination of soil available nutrient contents using multi-element hollow cathode lamp].

The soil available nutrient determination based on atomic absorption spectrometry using multi-element hollow cathode lamp (HCL) is improved from the instrument using single-element HCLs via modifying the software and hardware. As a test, available Cu, Fe, Zn, Mg and Ca contents of 30 fluvo-aquic soil samples measured by atomic absorption spectrometry using a multi-element HCL were compared with that measured by using single-element HCLs for 3 replications. A significant linear relationship with the slope close to 1 was found in soil available Cu, Fe, Zn and Ca contents measured by using multi-element HCL and single-element HCLs. The linear correlation coefficient of 0.86 and the slope of 0.85 were found in soil available Mg content. No significant difference was revealed from the above comparison data via analysis of variance. Therefore, the soil available nutrient determination based on atomic absorption spectrometry using multi-element HCL has the same measurement accuracy and is 50%-60% time-saving compared to that by using single-element HCLs.