改进的同时测定法测定混合染液各组分浓度

针对常规同时测定法存在测定周期长且对于多峰吸光度曲线不适用的问题,提出一种改进的同时测定法测定混合染液中各组分的浓度。首先运用高斯逼近法拟合固定浓度下各单一染液的吸光度、波长的模型。然后根据朗伯-比尔定律推导出各单一染液的吸光度、波长与浓度的模型,并给出了求混合染液各组分含量的具体步骤。最后以3种活性染料的混合染液浓度测定说明算法的可行性和有效性。

微孔滤膜中16种金属及其可溶性化合物电感耦合等离子体质谱同时测定法

目的建立微孔滤膜中镉、铬、锰、锌、铜、铁、钙、镁、铯、铟、锶、铋、锗、钽、锆和锡16种金属及其可溶性化合物同时测定的职业卫生检测方法。方法采用微孔滤膜采集工作场所空气中的16种金属及其可溶性化合物,硝酸溶液消解后转移至比色管定容,电感耦合等离子体质谱(inductively coupled plasma-mass spectrometry,ICP-MS)法同时测定16种金属及其可溶性化合物的质量浓度。结果16种金属元素在0.00~1000.00 g/L范围内线性关系良好,曲线的相关系数为0.9997~1.0000,检出限为0.10~3.11 g/L,定量下限为0.33~10.36 g/L;最低检出浓度为0.01×10^(-3)~0.41×10^(-3)mg/m3,最低定量浓度为0.06×10^(-3)~1.38×10^(-3)mg/m^(3)(以现场采集75 L空气样品来计算);加标回收率为96.41%~104.18%,相对标准偏差为0.14%~3.14%;样品在室温下至少可稳定保存7 d再进行消解和测定。结论本方法可优化程序和提高工作效率,并符合工作场所空气中化学物质测定方法的研制规范,可用于工作场所空气中镉、铬、锰、锌、铜、铁、钙、镁、铯、铟、锶、铋、锗、钽、锆、和锡16种金属及其可溶性化合物的同时测定。

溴代苯基荧光酮分光光度法同时测定人体血浆中的痕量锗和锌

研究了在溴化十六烷基三甲基铵(CTMAB)的存在下,溴代苯基荧光酮(BPF)与锗和锌反应分别形成稳定的络合物,可用来同时测定Ge4+和Zn2+。锗和锌络合物的最大吸收波长分别在540和565 nm处,摩尔吸光系数分别为1.66×105和4.35×104L.mol-1.cm-1。并利用k系数法进行校正避免Ge4+和Zn2+之间的干扰,用于人体血浆中锗、锌的测定。

矿物包裹体中气相组分的色谱法同时测定方法研究

文章提出以载气热爆—气相色谱法同时测定矿物包裹体中气相组分的方法。经对ＳＣ－３Ａ型气相色谱仪改装，并利用其改装后新的三柱串联双检测系统进行了一系列分离条件试验选择。对所选样品的分析、检验，表明所测结果可靠。

UPLC-MS/MS法同时测定一清颗粒中5种成分的含量

目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定一清颗粒中大黄素、大黄酚、大黄素甲醚、黄芩苷及盐酸小檗碱的含量方法。方法:采用ACQUITY UPLC BEN C_(18)色谱柱(50 mm×2.1 mm,1.7μm),流动相为乙腈-水(含0.1%甲酸),梯度洗脱;电喷雾离子源(ESI),正、负离子切换,多反应监测模式(MRM)。结果:5种成分在对应的线性范围中具有良好的线性关系,样品回收率在86.13%~96.37%(n=6),RSD在2.19%~3.03%。结论:该方法操作简单,定量准确,灵敏度高,可适用于一清颗粒中5种成分的质量控制。

河北电科院发明专利首获国家电网专利奖二等奖

3月12日，河北电科院一项发明专利“一种变压器油中多种金属元素的同时测定法”荣获国家电网公司专利奖二等奖，这是河北电力系统首次获得该殊荣。

Simultaneous Determination of Ceftazidime and Tazobactam in Injectable Powder by Reversed-Phase High Performance Liquid Chromatography

A reversed-phase high performance liquid chromatographic (RP-HPLC) method wasdeveloped and validated for the simultaneous deteimination of ceftazidime and tazobactam ininject-able powder. Methods Chromatography was carried out on Zorbax 300SB-C_(18) column using amixture of methanol and aqueous solution of phosphate buffer (pH = 5.6) as mobile phase. The UVdetection wavelength was 220 run. Results The linear ranges of ceftazidime and tazobactam were 0.62- 631.8 μg·mL^(-1) and 0.66 - 677.50 μg·mL^(-1), respectively. The average recoveries were 98.8%- 101.4% for ceftazidime, and 99,1% - 100.2% for tazobactam. The RSD values of inter-day andintra-day assays were lower than 1.5% for ceftazidime and 2.6% for tazobactam. Conclusion Thismethod is reproducible, simple, precise, and rapid for the quality control of ceftazidime andtazobactam in injectable powder.

Simultaneous separation and determination of four main isoflavonoids in Astragali Radix by an isocratic LC/ESI-MS method

A simple, reliable and rapid isocratic liquid chromatography(LC)-mass spectrometric detection(MS) coupled with electrospray ionization(ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-glucoside, ononin, calycosin and formonometin in Astragali Radix was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using water and acetonitrile(70:30, v/v) containing 0.2%(v/v) acetic acid as a mobile phase and a 2.0 mm×150 mm Hypersil-Keystone C18 column. Selective ion monitoring(SIM) mode and [M+H]+ ions at m/z 447, 431, 285 and 269 were used for quantitative analysis of four main active components above mentioned. The calibration curves were linear in the range of 0.4-175.0 μg/mL for calycosin-7-O-β-D-glucoside, 0.2-146.0 μg/m L for ononin, 0.4-210.0 μg/mL for calycosin and 0.5-217.0 μg/mL for formonetion, respectively. The limits of quantification(LOQ) and detection(LOD) were 0.4 μg/mL and 0.08 μg/m L for calycosin-7-O-β-D-glucoside, 0.2 μg/mL and 0.06 μg/m L for ononin, 0.4 μg/mL and 0.1 μg/mL for calycosin, 0.5 μg/m L and 0.1 μg/m L formonetion, respectively. The standard recoveries were in the range of 96.5%-104.7%. The developed method has successfully been used for the determination of four main flavonoids in Astragali Radix from various sources and can be used for identification, differentiation and quality evaluation of Astragali Radix.

Simultaneous Determination of Saponins in Radix Glycyrrhizae, Notoginseng and Ginseng by High Performance Liquid Chromatography

To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.

Simultaneous determination of brilliant blue and indigotine by derivative fluorescence spectrometry combined with WT-RBFNN

The mixed solutions of brilliant blue and indigotine are prepared and the fluorescence spectra of them are experimentally measured. The serious overlapping spectra of brilliant blue and indigotine are solved by means of the first-derivative fluorescence spectrometry. The wavelet coefficients, obtained by compressing the spectral data using wavelet transformation （WT）, are taken as inputs to establish the radial basis function neural network （RBFNN）. The neural network model can realize simultaneous determination of brilliant bFue and indigotine, and the mean relative errors of both compounds are 1.84% and 1.26%, respectively

HPLC-DAD data coupled with second-order calibration method applied to food analysis: Simultaneous determination of six benzoylurea insecticides in various fruit samples by selecting time region of chromatogram

This work presents a novel application of second-order calibration based on self-weighted alternating trilinear decomposition(SWATLD)algorithm for analyzing the HPLC-DAD data.The proposed method makes it possible to simultaneously determine teflubenzuron,hexaflumuron,flufenoxuron,chlorfluazuron,diflubenzuron and benzoylurea in different fruit samples,i.e.pear,apple and banana,in the selected time region of chromatogram.The concentration,elution time and spectral information of these benzoylurea insecticides are selectively extracted from complex matrices even in the presence of unknown interferences.The root-mean-square error of prediction(RMSEP)and figures of merit,including sensitivity(SEN),selectivity(SEL)and limit of detection(LOD)are employed to access the performance of the method.The LODs obtained for these insecticides are within the range 0.017–0.26 ppm in pears,0.039–0.33 ppm in apples,0.041–0.44 ppm in bananas,respectively.Such a chemometrics-based protocol holds great potential to be extended as a promising alternative for more practical applications in food safety and quality monitoring.