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用导数分光光度法测定二元混合物及加标人血清中的索他洛尔、氧烯洛尔和拉贝洛尔。

DETERMINATION OF SOTALOL, OXPRENOLOL AND LABETALOL IN BINARY MIXTURES AND IN SPIKED HUMAN SERUM BY DERIVATIVE SPECTROPHOTOMETRIC METHOD.

作者信息

Stolarczyk Mariusz, Apola Anna, Malanka Anna, Kwiecien Anna, Wrona Edyta, Opoka Wlodzimierz

出版信息

Acta Pol Pharm. 2017 Jan;74(1):93-102.

Abstract

The usefulness of derivative spectrophotometry for the determination of labetalol, sotalol and oxprenolol in binary mixtures and in human spiked serum was checked. To this aim a spectrophotometric analysis of samples in the UV range was carried out and the obtained results revealed that derivative spectropho- tometry allows for the fast, accurate and precise determination of the tested substances in spite of their clear interference in the zero-order spectra. For quantitative determinations "zero-crossing" technique was used to establish wavelengths for zeros of specified component. In a mixture of labetalol and oxprenolol the following wavelengths were established: D1 λ = 245.32 nm and 266.03 nm, D2 λ = 243.30 nm and 301.09 nm. respectively. D3 derivative did not show zeros suitable for quantitative analysis. For the analysis of labetalol and sotalol mixture, D3 derivative spectrophotometry was used at the following wavelengths: = 246.03 nm and λ = 249.91 rum, respectively. In this case, the curves of Dl and D2 derivatives showed no zeros that can be used in quantitative analysis. To determine the concentration of the components in a mixture containing oxprenolol and sotalol the following wavelengths were selected: for oxprenolol DI λ = 245.32 nm, D2 λ = 240.18 run, D3 λ = 232.05 nm and for sotalol Dl λ = 230.56 nm, D2 Xλ= 232.65 nm and D3 X = 238.84 tm, respectively. The developed spectrophotometric method was characterized by high sensitivity and accuracy, LOD determined for sotalol was in the range of 0.21-1.88 μg/mL, for labetalol 1.00-3.43 μg/mL and for oxprenolol 0.16-2.06 μg/mL; LOQ determined for sotalol was in the range of 0.65-5.70 μg/mL, for labetalol 3.11-10.39 μg/mL and for oxprenolol 0.47-6.23 μg/mL, depending on the composition of the tested mixture and the order of the deriv- ative. The recovery of the individual components was within the range of 100 ± 5%. The linearity range was wide and estimated for sotalol in the range of 11.00-38.50 μg/mL, for labetalol 12.80-44.80 μg/mL and for oxprenolol 12.60-44.10 μg/mL with correlation coefficients in the range of 0.9977-0.9999.

摘要

考察了导数分光光度法用于测定二元混合物及加标人血清中拉贝洛尔、索他洛尔和氧烯洛尔的实用性。为此,对样品在紫外范围内进行了分光光度分析,所得结果表明,尽管被测物质在零级光谱中有明显干扰,但导数分光光度法仍能快速、准确且精确地测定这些物质。对于定量测定,采用“零交叉”技术确定特定组分零值的波长。在拉贝洛尔和氧烯洛尔的混合物中,确定的波长如下:一阶导数λ = 245.32 nm和266.03 nm,二阶导数λ = 243.30 nm和301.09 nm。三阶导数未显示出适用于定量分析的零值。对于拉贝洛尔和索他洛尔混合物的分析,三阶导数分光光度法在以下波长下使用:λ = 246.03 nm和λ = 249.91 nm。在这种情况下,一阶和二阶导数曲线未显示可用于定量分析的零值。为了测定含有氧烯洛尔和索他洛尔混合物中各组分的浓度,选择了以下波长:对于氧烯洛尔,一阶导数λ = 245.32 nm,二阶导数λ = 240.18 nm,三阶导数λ = 232.05 nm;对于索他洛尔,一阶导数λ = 230.56 nm,二阶导数λ = 232.65 nm,三阶导数λ = 238.84 nm。所建立的分光光度法具有高灵敏度和准确性,索他洛尔的检测限在0.21 - 1.88 μg/mL范围内,拉贝洛尔为1.00 - 3.43 μg/mL,氧烯洛尔为0.16 - 2.06 μg/mL;索他洛尔的定量限在0.65 - 5.70 μg/mL范围内,拉贝洛尔为3.11 - 10.39 μg/mL,氧烯洛尔为0.47 - 6.23 μg/mL,具体取决于被测混合物的组成和导数阶数。各组分的回收率在100 ± 5%范围内。线性范围较宽,索他洛尔的线性范围估计为11.00 - 38.50 μg/mL,拉贝洛尔为12.80 - 44.80 μg/mL,氧烯洛尔为12.60 - 44.10 μg/mL,相关系数在0.9977 - 0.9999范围内。

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