目的建立高效液相色谱-串联质谱法测定安神类保健品中巴比妥残留的分析方法。方法样品经甲醇-水溶液(50:50, V:V)超声提取、离心、过膜后,经C18色谱柱(50 mm×2.1 mm, 2.6μm)分离,以水和乙腈作为流动相,梯度洗脱。在负电喷雾离子...目的建立高效液相色谱-串联质谱法测定安神类保健品中巴比妥残留的分析方法。方法样品经甲醇-水溶液(50:50, V:V)超声提取、离心、过膜后,经C18色谱柱(50 mm×2.1 mm, 2.6μm)分离,以水和乙腈作为流动相,梯度洗脱。在负电喷雾离子模式下,采用多反应监测模式检测。结果巴比妥在液体和固体基质中的绝对基质效应为4.97%~69.36%,在1.0~50.0 ng/mL范围内线性均良好,相关系数(r^(2))均在0.998以上。巴比妥在0.1、0.5和1.0μg/g3个水平的加标回收率为96.2%~112.0%,相对标准标准偏差为0.10%~6.3%(n=6)。结论本方法操作简单、高效、可靠、灵敏度高,能满足安神类保健品市场的监管和检验需求。展开更多
Monte Carlo方法是一种数值计算方法。它既能求解确定性的数学问题,又能求解随机性的问题。本文应用Monte Carlo面积拟合算法,用微机对安痛定注射液的紫外光谱数据进行处理,不经分离测定了该制剂的巴比妥、氨基比林、安替比林三组分含...Monte Carlo方法是一种数值计算方法。它既能求解确定性的数学问题,又能求解随机性的问题。本文应用Monte Carlo面积拟合算法,用微机对安痛定注射液的紫外光谱数据进行处理,不经分离测定了该制剂的巴比妥、氨基比林、安替比林三组分含量。平均回收率分别为99.1±1.1(CV);99.6±1.3(CV)和99.7±1.0%(CV)。展开更多
Some biologically important tin（Ⅳ） complexes derived from 5,5-diethyl sodium barbital have been synthesized and characterized through various analytical and spectroscopic techniques such as IR, ^1H-, ^13C-NMR and ^...Some biologically important tin（Ⅳ） complexes derived from 5,5-diethyl sodium barbital have been synthesized and characterized through various analytical and spectroscopic techniques such as IR, ^1H-, ^13C-NMR and ^119mSn mossbauer. On the basis of these spectroscopic techniques, octahedral geometry has been assigned to all the novel compounds. These complexes, soluble in DMSO and DMF, were screened against a wide range of microorganisms. The results proved that the diphenyltin（Ⅳ） and dibutyltin（Ⅳ） complexes exhibit excellent activity against all types of microorganisms, while the rest of the compounds show significant activity that can be used during the biological study.展开更多
A molecularly imprinted electrochemical sensor was prepared based on poly folic acid（PFA） for rapid detection of barbital（BAR）. The PFA membrane was obtained via directly electropolymerization technique on the sur...A molecularly imprinted electrochemical sensor was prepared based on poly folic acid（PFA） for rapid detection of barbital（BAR）. The PFA membrane was obtained via directly electropolymerization technique on the surface of chemically modified Au electrode（Au/CME） by means of cyclic voltammetry（CV） in the potential range between-0.4 and 1.0 V in phosphate buffer solution（PBS） pH 7.04. The molecularly imprinted polymers（MIP） membrane was synthesized with BAR as template molecules and folic acid（FA） as the functional monomer. The performance and surface feature of the proposed imprinted sensor were investigated using CV, differential pulse voltammetry（DPV）, electrochemical impedance spectroscopy（EIS） and scanning electron microscope（SEM）. Under the optimized conditions, the peak current decrease（ΔIp） was proportional to the BAR concentration in the range of 1.00×10^-7-1.00×10^-4 mol/L（R^2=0.998 2） with a detection limit（S/N=3） of 4.65×10^-8 mol/L. The results indicated that the imprinted sensor exhibited an excellent selectivity for BAR and it was successfully used to determine BAR in real samples with recoveries of 94.7%-106.2% by using the standard addition method.展开更多
文摘Some biologically important tin（Ⅳ） complexes derived from 5,5-diethyl sodium barbital have been synthesized and characterized through various analytical and spectroscopic techniques such as IR, ^1H-, ^13C-NMR and ^119mSn mossbauer. On the basis of these spectroscopic techniques, octahedral geometry has been assigned to all the novel compounds. These complexes, soluble in DMSO and DMF, were screened against a wide range of microorganisms. The results proved that the diphenyltin（Ⅳ） and dibutyltin（Ⅳ） complexes exhibit excellent activity against all types of microorganisms, while the rest of the compounds show significant activity that can be used during the biological study.
基金Supported by the Natural Science Foundation of Shanxi Province(20001057)
文摘A molecularly imprinted electrochemical sensor was prepared based on poly folic acid（PFA） for rapid detection of barbital（BAR）. The PFA membrane was obtained via directly electropolymerization technique on the surface of chemically modified Au electrode（Au/CME） by means of cyclic voltammetry（CV） in the potential range between-0.4 and 1.0 V in phosphate buffer solution（PBS） pH 7.04. The molecularly imprinted polymers（MIP） membrane was synthesized with BAR as template molecules and folic acid（FA） as the functional monomer. The performance and surface feature of the proposed imprinted sensor were investigated using CV, differential pulse voltammetry（DPV）, electrochemical impedance spectroscopy（EIS） and scanning electron microscope（SEM）. Under the optimized conditions, the peak current decrease（ΔIp） was proportional to the BAR concentration in the range of 1.00×10^-7-1.00×10^-4 mol/L（R^2=0.998 2） with a detection limit（S/N=3） of 4.65×10^-8 mol/L. The results indicated that the imprinted sensor exhibited an excellent selectivity for BAR and it was successfully used to determine BAR in real samples with recoveries of 94.7%-106.2% by using the standard addition method.
