分光光度法测定新鲜蔬菜中维生素C的含量

水溶性的维生素C是一种人体必需的营养物质。维生素C是含有烯二醇基的多羟基内酯结构,利用其水溶液在波长265nm处有较强烈的紫外吸收峰,建立了直接用紫外分光光度法测定新鲜蔬菜中维生素C含量的方法。实验结果表明,维生素C的含量在1.0~12.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%~105.4%。方法操作简单,准确度高,对新鲜蔬菜的测定结果令人满意。     

紫外分光光度法测定聚硫密封胶中二氧化钛

基于强酸性溶液中钛氧离子与H2O2发生显色络合反应的原理,建立了浓硫酸–硫酸铵消解–紫外分光光度法测定聚硫密封胶中TiO_2含量的方法。通过对酸液和显色剂用量,以及显色络合物稳定性的系统考察,确定浓硫酸用量为2 mL,双氧水用量为3 mL,检测波长为403 nm。二氧化钛质量浓度在0~130μg/mL范围内与其吸光度呈良好的线性关系,线性方程为A=5.047 8c–0.019 31,r~2=0.999 2,检出限为0.08μg/mL。检测结果的相对标准偏差为0.89%(n=5),3水平加标平均回收率为101.7%。该方法线性范围较宽、检出限低、重复性好,可用于聚硫密封胶中二氧化钛的定量分析。     

丝瓜中维生素C含量的测定

为建立丝瓜中维生素C含量直接测定的新方法,以10%盐酸溶液为溶剂,采用紫外分光光度法测定其含量。结果表明,维生素C在0～10 mg/L质量浓度范围内与吸光度呈良好的线性关系,回归方程为:y=0.047 46ρ+0.001 09,r=0.999 7。检出限为0.023μg/mL,加标回收率在90.6%～99.0%之间。该法操作简单,结果准确,应用于维生素C含量的测定,结果准确,令人满意,可作为控制维生素C质量的方法。     

柱前衍生高效液相色谱法测定甘草中甘草酸含量

建立了柱前衍生高效液相色谱测定甘草中甘草酸的新方法。以对硝基溴化苄为柱前衍生化试剂,采用Phenomenex C18分离,以乙腈-3%冰乙酸溶液(体积比60∶40)为流动相,紫外290nm检测。结果表明,在10.0～100.0μg/mL浓度范围内,甘草酸衍生物的峰面积与甘草酸浓度呈现良好的线性关系,相关系数为0.9951,相对标准偏差为2.1%(c=30.0μg/mL,n=6),检出限为1.0μg/mL,加标回收率为96.7%～101.1%。该法准确,灵敏度高,已用于甘草中甘草酸含量的测定。     

分光光度法测定丙烯酸及丙烯酸酯中阻聚剂的含量

采用乙醇作溶剂,亚硝酸钠作显色剂,用分光光度法于400 nm处对丙烯酸及丙烯酸酯中阻聚剂含量进行测定。阻聚剂含量y在0~120μg/(25 mL)范围内与吸光度x呈线性关系,线性方程为y=1 768.5x-15.123,r=0.999 5。方法检出限为0.1μg/mL,测定结果的相对偏差为2.26%~2.91%(n=5)。加标回收率为96.5%~100.7%。     

微波消解-原子荧光光谱法测定化妆品中的砷

建立了微波消解-原子荧光光谱法测定化妆品中微量砷的方法.砷浓度在0～50.00μg/L范围内与荧光强度呈线性关系,线性方程为,If=56.5486c,相关系数r=0.9993,砷的检出限为0.084μg/L.砷测定结果的相对标准偏差为1.49%(n=6),加标回收率为90.7%～107.5%.用该法对环境标准样品进行测定,结果与标准值相吻合.     

荧光分析法测定维生素C

维生素C经Cu2 氧化为脱氢抗坏血酸,与苯甲酸及十六烷基三甲基溴化铵产生荧光协同增敏作用。提出一种新的测定维生素C的高灵敏荧光分析法,建立了测定维生素C的适合条件。该方法的的线性范围为0.02~8.0μg/mL,检出限为0.006 5μg/mL。对3.0μg/mL的维生素C测定6次,测定结果的相对标准偏差为0.12%。将该法用于西红柿、果珍以及维生素C药片中维生素C含量的测定,加标回收率为96.7%~100.5%。     

HPLC法测定党参中烟酸和党参炔苷的含量

建立HPLC法同时测定党参中烟酸及党参炔苷含量的方法。采用Syncronis AQ色谱柱(250 mm×4.6mm,5μm),以乙腈(A)–0.2%磷酸水溶液(B)作流动相进行梯度洗脱,流量为1 mL/min,紫外检测波长为285 nm,柱温为30℃,烟酸和党参炔苷可在24 min内实现与其它成分良好分离。烟酸的质量浓度在9.6~57.6μg/mL范围内与色谱峰面积线性关系良好(r=0.999 2),检出限为0.94μg/mL,测定结果的相对标准偏差为1.5%(n=6),平均加标回收率为99.5%;党参炔苷的质量浓度在9.92~59.52μg/mL范围内与色谱峰面积线性关系良好(r=0.999 6),检出限为0.12μg/mL,测定结果的相对标准偏差为1.9%(n=6),平均加标回收率为101.1%。该方法操作简便、快速、准确,具有良好的重复性,可作为党参中烟酸、党参炔苷测定的有效方法。     

水发食品中痕量甲醛的测定

为建立催化动力学荧光法测定痕量甲醛的新方法,基于在酸性介质中,甲醛催化KBrO3氧化藏红T的褪色反应,使其荧光猝灭的原理,将反应体系在沸水浴中加热8 min,流水冷却3min,采用动力学荧光法测定痕量甲醛。结果表明,甲醛在0.02~0.14μg/mL范围内与△F值呈良好的线性关系,线性方程为△F=-1.642 8+274.12C(μg/mL),r=0.996 9,检出限为0.011μg/mL。该法简便,快速,常见共存物质干扰小,可用于水发食品及其它食品中甲醛含量的测定,加标回收率为84.63%~94.93%。     

碘量紫外分光光度法测定碳氢燃料过氧化值

建立测定碳氢燃料过氧化值的碘量紫外分光光度法。样品溶于乙醇中，加入0.50 mL冰乙酸，用饱和碘化钾-乙醇溶液定容至10 mL，避光显色90 min，过氧化物在酸性条件下与碘化钾反应生成黄色的I₃^-，在360 nm处测定吸光度，计算过氧化氢的含量。过氧化氢的质量浓度在0.106 1～1.061μg/mL范围内与吸光度线性关系良好，相关系数为0.999 8，方法检出限为0.015μg/mL。样品加标回收率为97.3%～103.6%，测定结果的相对标准偏差小于5%(n=6)。该法适用于测定碳氢燃料的过氧化值。     

高效液相色谱法测定强化食品中维生素C的含量

建立了强化食品(饮料、奶粉、含乳饮料、大米、果泥及果冻)中维生素C含量的高效液相色谱检测方法。优化了样品处理方法,在水浴控温和避光条件下处理样品,避免维生素C被氧化。选用Tech Mate C18–ST(250 mm×4.6 mm,5μm)反相色谱柱,以0.05 mol/L磷酸二氢钾缓冲溶液(p H 3)为流动相,流量为1.0m L/min,检测器为光电二极管阵列检测器,检测波长为266 nm。线性范围为0.2~100μg/m L,相关系数为0.999 6,果泥中维生素C的定量限为20 mg/kg,其它为100 mg/kg,加标回收率为82.2%~107%,测定结果的相对标准偏差为1.23%~6.86%(n=8)。该方法简单快速,其灵敏度、准确度和精密度均能满足强化食品中维生素C的检测要求。     

First-order Derivative Spectrophotometry for the Determination of Vitamin C in Medicament

A novel method for the determination of vitamin C（Vc） is proposed in this article. After the reaction with Folin-Ciocalteau reagent at ambient temperature, Vc solution was scanned at 750--1100 nm, and its first-order derivative spectrum were obtained from the original spectrum. The values of derivative selected at 995 nm were used for determination. It was proved that Vc could quickly react with Folin-Ciocalteau reagent within 5 min and the product was quite stable for a long time. The conditions required for this method is not very complicated, its precision and accuracy are similar to those of the iodometric titration described in Chinese Pharmacopoeia, and the limit of detection is 0.312 μg/mL. The determination of the results of vitamin C tablet, pill, and injection demonstrates that this method has wide pharmaceutical applications.     

怀药中维生素C含量的测定

为建立怀药中维生素C含量直接测定新方法,以pH 2.5硫酸溶液为溶剂,采用紫外分光光度法测定了怀药中维生素C含量.结果表明,维生素C在0～15 μg/mL范围内与吸光度呈良好的线性关系,回归方程为:y=0.060 29 C+0.003 55,r=0.999 9,所选的怀药均含丰富的维生素C,其中怀菊花中高达 51.55...     

高效液相色谱法同时测定长春花中的文多灵、长春质碱和脱水长春碱

运用高效液相色谱（HPLC）梯度洗脱同时测定了长春花中的文多灵、长春质碱和脱水长春碱等3种生物碱。色谱柱为Waters 5C18-MS-Ⅱ(4.6 mm×250 mm),流动相为甲醇-1%二乙胺(磷酸调pH至7.3)系统,梯度洗脱,检测波长220 nm,柱温25 ℃。实验结果表明,文多灵、长春质碱和脱水长春碱等3种生物碱分别在0.03～1 mg/mL,0.03～1 mg/mL和0.01～0.5 mg/mL时线性关系良好,平均加样回收率分别为96.8%,97.0%和96.4%,相对标准偏差(RSD)分别为1.53%,1.37%和1.96%。用该法同时检测了不同干旱条件处理下长春花样品中的文多灵、长春质碱和脱水长春碱,方法准确、快速、简便。     

Indirect Determination of Ascorbic Acid with Ammonium Sulfate and Isopropyl Alcohol by Extraction-flotation of Copper

A new method of indirect determination of ascorbic acid(Vc) with ammonium sulfateand isopropyl alcohol by extraction-flotation of copper is studied in this paper. It shows that asmall amount of Cu( II ) can be reduced to Cu( I ) by Vc, then Cu( I ) reacted with the SCN-,which precipitated on the interface of isopropyl alcohol and H2O. A good linear relationshin is observed between the flotation yield(E) of Cu( II ) and the amount of Vc. The detection limi(forVc is 1.76 μg/mL. The method is simple, rapid (5 rain), but suffers from little interference of common anions and cations. It has been successfully applied for the determination of Vc in fruits.     

HPLC-F analysis of melatonin and resveratrol isomers in wine using an SPE procedure

An original analytical method has been developed for the determination of the antioxidants trans-resveratrol (t-RSV) and cis-resveratrol (c-RSV) and of melatonin (MLT) in red and white wine. The method is based on HPLC coupled to fluorescence detection. Separation was obtained by using a RP column (C8, 150 mm x 4.6 mm id, 5 mum) and a mobile phase composed of 79% aqueous phosphate buffer at pH 3.0 and 21% ACN. Fluorescence intensity was monitored at lambda = 386 nm while exciting at lambda = 298 nm, mirtazapine was used as the internal standard. A careful pretreatment of wine samples was developed, using SPE with C18 cartridges (100 mg, 1 mL). The calibration curves were linear over the following concentration ranges: 0.03-5.00 ng/mL for MLT, 3-500 ng/mL for t-RSV and 1-150 ng/mL for c-RSV. The LOD values were 0.01 ng/mL for MLT, 1 ng/mL for t-RSV and 0.3 ng/mL for c-RSV. Precision data, as well as extraction yield and sample purification results, were satisfactory. Thus, the method seems to be suitable for the analysis of MLT and resveratrol isomers in wine samples. Moreover, wine total polyphenol content and antioxidant activity were evaluated.     

Rapid and selective micellar electrokinetic chromatography for simultaneous determination of amikacin, kanamycin A, and tobramycin with UV detection and application in drug formulations

A simple and selective micellar electrokinetic chromatography (MEKC) with UV detection is described for simultaneous determination of amikacin, tobramycin, and kanamycin A, performed in Tris buffer (180 mM; pH 9.1) with 300 mM sodium pentanesulfonate (SPS) as an anionic surfactant. Under this condition, good separation with high efficiency and the required short analysis time is achieved. The linear ranges of the method for the determination of amikacin, tobramycin, and kanamycin A were 0.1-0.5 mg / mL, 0.4-2.0 mg / mL, and 0.4-2.0 mg / mL, respectively; the detection limits (signal-to-noise ratio = 3; injection, 0.5 psi 5 s) were 0.08, 0.2, and 0.2 mg / mL, respectively. The small amount of sample required and the expeditiousness of the procedure allow content uniformity to be determined in individual commercial products.     

火焰原子吸收光谱法测定锌合金中镁

建立火焰原子吸收光谱法测定锌合金中镁含量。选用10 mL盐酸溶液(1+1)溶解样品,加入5 mL质量浓度为100 g/L的LaCl3溶液,以消除铝对镁的化学干扰,在选定的仪器工作条件下进行测定。结果表明,镁的质量浓度在0~1.238 mg/L范围内与与吸光度具有良好的线性关系,相关系数为0.999 4,线性方程为Y=1.086 4X+0.018 5,方法测定下限为0.010 mg/L。样品测定结果的相对标准偏差为1.61%~3.45%(n=6),加标回收率为91.3%~94.7%。该方法准确度高,精密度好,满足锌合金中镁含量的日常检测要求。     

高效液相色谱法测定肉制品中甘草抗氧化物的含量

建立了测定肉制品中甘草抗氧化物含量的方法。样品经流动相提取,采用C．8色谱柱分离,以甲醇-0．2mol／L乙酸铵-冰乙酸（体积比70：29：1）为流动相,流速为1．0mL／min,波长为250nm,以保留时间进行定性,峰面积进行定量。甘草酸在1．0-80．0μg／mL范围内线性关系良好,回归方程为y=8．55×10^-5x-0．599（r=0．9997）,检出限为1．0mg／kg,定量限为3．0mg／kg,加标回收率为95．7％-103．4％,测定结果的相对标准偏差为1．57％-3．53％（n=6）。该方法适用于检验机构日常检验中大批量肉制品中甘草抗氧化物含量的测定。