Effect of processing on folic acid fortified Baladi bread and its possible effect on the prevention of colon cancer

This paper studied the possible effect of folic acid in fortified Baladi bread on the prevention of colon cancer development in rats. Wheat flour samples (82% extraction rate) and soy bean flour were analyzed to determine their folic acid contents using the High Performance Liquid Chromatography (HPLC). Unfortified and folic acid fortified Baladi breads were prepared.     

HPLC法测定含有多种维生素类制剂中四种维生素含量

目的:建立HPLC法测定含有多种维生素类制剂中四种维生素(维生素B1、维生素B2、维生素B6、烟酰胺)的含量.方法:采用C18柱,以0.05mol/L己烷磺酸钠溶液(用冰醋酸调节pH值为3.0)-甲醇(80:20)为流动相,流速为1.0ml/min.紫外检测波长为254nm.结果:本实验中维生素B1、维生素B2、维生素B6、烟酰胺线性范围分别为4～20μg/ml(r=0.9997),4～20μg/ml(r=0.9998),0.8～4μg/ml(r=0.9997),32～160μg/ml(r=0.9999),方法的回收率在98.5%～100.4%,RSD为0.23%～1.10%.各组分间的分离度均符合要求.结论:本方法快速、简便、准确,分离效果好,辅料无干扰,适用于该类制剂中四种维生素组分同时测定.     

Polycyclic aromatic hydrocarbons incidence in Portuguese traditional smoked meat products

Meat and meat products safety is, nowadays, a priority quality requirement with chemical hazards having a great impact. Amongst the residues and contaminants, polycyclic aromatic hydrocarbons (PAHs) can be of particular concern, namely in those products having direct smoking during processing. In order to investigate the contamination levels in traditional dry fermented sausages manufactured in Alentejo (South of Portugal), 66 samples were collected from regional producers. PAH8 represented less than 0.5% of the total contamination profile, with benzo[a]anthracene and chrysene being the most concentrated compounds (maximum contents of 7.53 and 8.9 μg kg⁻¹), irrespective of the product type analysed. Benzo[a]pyrene content varied between 0.21 and 1.00 μg kg⁻¹, with only one sample showing this maximum content. Blood sausages were potentially more risky, since total PAH8 contents were generally higher and because its presence in inner parts were significantly superior than that found in casings, comparatively to meat counterparts, which expressed superior benzo[a]pyrene toxic equivalents.     

Effect of high pressure processing on cholesterol oxidation products in vacuum packaged sliced dry-cured ham

The effect of high pressure processing (at 600 and 900 MPa) on cholesterol oxidation products has been studied in vacuum packaged sliced dry-cured ham. Pressurisation of dry-cured ham at 600 MPa did not show changes in the contents of cholesterol oxidation products. However, the effect of pressurisation at 900 MPa produced a significant increase in the contents of 7α-hydroxycholesterol, 7β-hydroxycholesterol, β-epoxycholesterol, α-epoxycholesterol, 25-hydroxycholesterol and 7-ketocholesterol. In view of the results, at the pressure of 900 MPa, a strong damage of membrane could be produced and the potential production of harmful compounds in dry-cured ham as it was observed for cholesterol oxidation products.     

高效液相色谱法测定三维制霉素栓中维生素E含量

目的建立测定三维制霉素栓中维生素E含量的高效液相色谱法。方法色谱柱为Hypersil C18柱（250mm×4．6mm,5μm）,流动相为甲醇-水（90：10）,检测波长280nm,流速0．8mL／min。结果维生素E进样量在0．484～3．872μg范围内与峰面积呈良好的线性关系（r=0．9998）,平均回收率为99．62％,RSD为1．81％（n=6）。结论高效液相色谱法简便快捷,重现性好,可作为三维制霉素栓中维生素E的含量测定方法。     

反相高效液相色谱法同时测定四维钙片中多种维生素含量

目的对四维钙片中的维生素C（VitC）、维生素B1（vitB1）及维生素B2（VitB2）进行含量测定。方法采用反相高效液相色谱法，使用Zorbax Eclipse XDB—C8柱（150mm×4．6mm，5μm），流动相为0．05％乙酸溶液（含0．005mol／L己烷磺酸钠、1．3％三乙胺，用冰醋酸调节pH值至3．5）-甲醇（90：lO），检测波长为254nm。结果VitC，VitB1，，VitB2质量浓度分别在7～60μg／mL，1～10μg／mL，1～10μg／mL范围内与峰面积线性关系良好，r分别为0．9998，0．9997，0．9998（n=8）；平均回收率分别为100．3％，99．1％，98．5％，RSD分别为1．2％．1．5％．1．6％（n=9）。结论该方法准确、简单,能够有效控制制剂的质量。     

HPLC法同时测定多维元素片中维生素A和维生素E的含量

目的建立高效液相色谱(HPLC)法同时测定多维元素片中维生素A和维生素E的含量。方法采用C18色谱柱(250mm×4.6mm,5μm);流动相为甲醇-水(98∶2);流速为1.0mL·min-1;检测波长为265nm;柱温为25℃。结果维生素A和维生素E的线性关系良好,相关系数(r)均大于0.999 9;专属性强,维生素A、维生素E与药品中其他成分之间均有良好的分离度;稳定性和精密度良好,相对标准偏差(RSD值)均小于1.0%;回收率良好,回收率在91.07%~92.85%之间;稳定性能满足实验要求。结论该法可同时定性和定量分析多维元素片中的维生素A和维生素E,其方法的精密度、回收率和检出限能满足实际检测要求,可用于该制剂中维生素A和维生素E的监测。     

柱前衍生-高效液相色谱法测定七维牛磺酸口服溶液中牛磺酸的含量

目的:建立牛磺酸的含量测定方法。方法:采用柱前衍生-高效液相色谱法测定七维牛磺酸口服溶液中牛磺酸的含量,C18(5μm,150mm×4.6mm)色谱柱;磷酸盐缓冲液(pH 值7.0)-乙腈(80:20)为流动相;检测波长为360nm。结果:牛磺酸含量测定条件稳定,专属性强,测定结果准确,重现性好,在0.13～4.07μg范围内线性关系良好,相关系数为0.9996。平均回收率为99.89%,RSD=1.39%。结论:本方法可作为七维牛磺酸口服液中牛磺酸含量测定质量标准。     

Isolation and structure determination of oxidative degradation products of atorvastatin

Methods were developed for the preparation and isolation of four oxidative degradation products of atorvastatin. ATV-FX1 was prepared in the alkaline acetonitrile solution of atorvastatin with the addition of hydrogen peroxide. The exposition of aqueous acetonitrile solution of atorvastatin to sunlight for several hours followed by the alkalization of the solution with potassium hydroxide to pH 8–9 gave ATV-FXA. By the acidification of the solution with phosphoric acid to pH 3 ATV-FXA1 and FXA2 were prepared. The isolation of oxidative degradation products was carried out on a reversed-phase chromatographic column Luna prep C18(2) 10 μm applying several separation steps. The liquid chromatography coupled with a mass spectrometer (LC-MS), high resolution MS (HR-MS), 1D and 2D NMR spectroscopy methods were applied for the structure elucidation. All degradants are due to the oxidation of the pyrrole ring. The most probable reaction mechanism is intermediate endoperoxide formation with subsequent rearrangement and nucleophilic attack by the 5-hydroxy group of the heptanoic fragment. ATV-FX1 is 4-[1b-(4-Fluoro-phenyl)-6-hydroxy-6-isopropyl-1a-phenyl-6a-phenylcarbamoyl-hexahydro-1,2-dioxa-5a-aza-cyclopropa[a]inden-3-yl]-3-(R)-hydroxy-butyric acid and has a molecular mass increased by two oxygen atoms with regard to atorvastatin. ATV-FXA is the regioisomeric compound, 4-[6-(4-Fluoro-phenyl)-6-hydroxy-1b-isopropyl-6a-phenyl-1a-phenylcarbamoyl-hexahydro-1,2-dioxa-5a-aza-cyclopropa[a]inden-3-yl]-3-(R)-hydroxy-butyric acid. Its descendants ATV-FXA1 and FXA2 appeared without the atorvastatin heptanoic fragment and are 3-(4-Fluoro-benzoyl)-2-isobutyryl-3-phenyl-oxirane-2-carboxylic acid phenylamide and 4-(4-Fluoro-phenyl)-2,4-dihydroxy-2-isopropyl-5-phenyl-3,6-dioxa-bicyclo[3.1.0]hexane-1-carboxylic acid phenylamide, respectively. Quantitative NMR spectroscopy was employed for the assay determination of isolated oxidative degradation products. The results obtained were used for the determination of the UV response factors relative to atorvastatin.     

维生素类药物在肿瘤治疗中的应用

综述维生素类药物的抗肿瘤作用机制和药理作用以及在肿瘤靶向给药系统中的应用。维生素及其衍生物不仅具有良好的抗肿瘤活性和毒副作用小的特点，且有独特的肿瘤靶向性，如叶酸和生物素，其应用于肿瘤靶向给药系统，可大大提高药物疗效及减小药物毒副作用。     

HPLC法测定五维赖氨酸口服溶液中维生素C、维生素B6、烟酰胺的含量

目的建立HPLC法测定五维赖氨酸口服溶液中维生素C、维生素B6、烟酰胺的含量方法。方法采用AlltimaTMC18色谱柱,流动相:0.03mol·L-1磷酸氢二铵溶液(加入0.05%庚烷磺酸钠和0.2%三乙胺,用磷酸调节pH至3.0)-甲醇,梯度洗脱,检测波长:277nm,流速:1.0 mL·min-1,柱温:30℃。结果维生素C、维生素B6、烟酰胺分别在2.587~20.670μg(r=0.9999)、0.123~0.980μg(r=1.0000)、1.126~9.007μg(r=1.0000)范围内线性关系良好,平均回收率分别为100.00%(RSD=0.10%)、99.06%(RSD=0.28%)、99.67(RSD=0.31%)(n=9)。结论本法简便、准确、可靠,可用于五维赖氨酸口服溶液中维生素C、维生素B6、烟酰胺的质量控制。     

复合氨基酸胶囊中水溶性维生素的含量测定

目的:建立复合氨基酸胶囊中5种水溶性维生素的含量测定方法.方法:采用高效液相色谱法,用乙腈与庚烷磺酸钠-磷酸钠的水溶液(pH=3.0)为流动相,流速1.0ml·min-1,色谱柱为C18(4.6×250mm,5μm),柱温40℃,检测波长为280nm,进样量为20μl.结果:维生素Bl、维生素B2、维生素B6、维生素C和烟酰胺分别在24.7～75.2μg·ml-1、15.0～44.9μg·ml-1、12.2～37.5μg·ml-1、99.2～299.9μg·ml-1和100.3～300.9μg·ml-1范围内呈线性关系,相关系数均为1.000,平均回收率均在100%±2%范围以内.RSD分别为0.19%、0.26%、0.46%、1.17%和0.52%.结论:本方法准确,简便,快捷,可以同时测定复合氨基酸胶囊中维生素B1、维生素B2、维生素B6、维生素C和烟酰胺的含量.     

黄芩炮制品生物检定法实验研究

目的研究黄芩炮制品对敏感菌株的剂量效应曲线,建立生物检定质量评价方法。方法利用黄芩炮制品提取液对敏感菌的抑菌圈直径大小和质量浓度的对数建立标准曲线,根据量效曲线测定不同产地、不同批号黄芩炮制品的相对效价。采用《中国药典》2010年版HPLC方法进行含量测定,比较生物检定法和药典方法是否一致。结果当黄芩炮制品的质量浓度在0.204 8～0.976 6g·mL-1范围内时,黄芩炮制品的对数剂量和反应效应呈线性关系,且相关性好(r=0.997 5);生物检定法和HPLC作为质控指标得出质量评价结果不完全相同。结论采用生物检定法建立黄芩炮制品质量控制方法是可行的、合理的。     

Photochemical fluorimetric analysis of phenylbutazone and its degradation products

A room temperature photochemical spectrofluorimetric (RTPF) method has been developed for the assay of phenylbutazone (PB), and its major degradation products. Fluorescence spectral properties of PB, its degradation products, and their photoproducts are reported, as well as the optimal irradiation times (ranging from 4 to 45 min), which correspond to maximum fluorescence signals of photoproducts. Linear log—log calibration plots were obtained over a 50- to 1000-fold range of concentration, and limits of detection ranged between 1 ng/ml and 1.2 μg/ml. This has been shown to be a convenient technique, in terms of simplicity, short measurement times, sensitivity, and precision.     

葫芦素B对肝癌细胞内阿霉素浓度的影响

目的建立肝癌细胞H22和HepG2中阿霉素含量测定的高效液相色谱方法,以明确葫芦素B对阿霉素在细胞内浓度的影响。方法色谱柱为Waters Sunfine C18柱(4.6 mm×150 mm,5μm),流动相为甲醇-0.01%醋酸(40∶60,V/V),流速为1.0 mL/min,柱温为30℃,荧光检测激发波长为495 nm,发射波长为560 nm,以盐酸表阿霉素为内标。结果在HepG2细胞液中,阿霉素线性范围为0.1～6.4μg/mL(r=0.993 4,n=7),加样回收率为107.4%,RSD为3.77%;在H22细胞液中,阿霉素线性范围为0.625～20μg/mL(r=0.996,n=7),加样回收率为105.93%,RSD为5.64%。结论在肝癌细胞中,葫芦素B能明显促进阿霉素内流,减少外排。葫芦素B使肝癌细胞中阿霉素的浓度升高,两者联合可能起到更好的抗肝癌作用,葫芦素B可能逆转肝癌细胞的阿霉素耐药性。     

HPLC法测定维他参颗粒中维生素B1的含量

目的建立维他参颗粒中维生素B1含量测定方法，为维他参颗粒质量标准的研究提供科学依据。方法采用高效液相色谱法测定维他参颗粒中维生素B1的含量。色谱条件为Agilent XDB-C18（5μm 150mm×4．6mm）色谱柱，以乙腈-0．008mol／L己烷磺酸钠-三乙胺-冰醋酸（12：87：0．25：0．75）为流动相；检测波长为246nm。结果此方法线性良好，平均加样回收率为99．8％，RSD为2．0％。结论本方法精密度高，分离度良好，可用于测定维他参颗粒中维生素B1的含量。     

HPLC法同时测定五维赖氨酸口服溶液中4种水溶性主成分的含量

目的:建立直接同时测定五维赖氨酸口服溶液中盐酸赖氨酸和三种水溶性维生素含量的RP-HPLC法。方法:采用Phenomenex Gemini C₁₈ 100A(4.6 mm×250 mm, 5μm)色谱柱，以0.03 mol·L^-1磷酸二氢铵溶液(pH 3.0)-甲醇(98∶2)为流动相，检测波长为205 nm,流速1.0 mL·min^-1。结果:盐酸赖氨酸、维生素C、维生素B₆和烟酰胺分别在30.56～488.9μg·mL^-1(r=1.000 0)、24.86～397.8μg·mL^-1(r=0.999 8)、1.018～16.29μg·mL^-1(r=1.000 0)、10.72～171.5μg·mL^-1(r=0.999 0)范围内与峰面积呈良好的线性关系；定量限分别为10.39、0.466 1、0.092 79、0.136 2 ng;平均回收率分别为100.6%、98.5%、98.0%、99.2%,RSD分别为0...     

HPLC测定保健品中西地那非的含量

目的 对保健品中掺入的西地那非进行定量分析。方法 采用HPLC法,固定相用CLC-ODS柱,流动相为0.05 mol·L-1三乙胺(磷酸凋pH 3.0±0.1)-甲醇-乙腈(50∶30∶20),检测波长290nm。结果 线性范围为0.05-2.0 mg·ml-1,r=0.9994;12批样品中,西地那非每粒的含量为15～81 mg。结论 该方法可用于保健品中西地那非的含量测定。目前,性保健品中掺入西地那非的现象应引起足够重视。     

HPLC法测定五维葡钙口服溶液中四组份的含量

目的:建立HPLC法同时测定五维葡钙口服溶液中维生素B1,维生素B2,维生素B6(以下简称VB1,VB2,VB6)和烟酰胺的含量.方法:采用C18柱;以0.005 mol·L-1己烷磺酸钠与0.008 mol·L-1庚烷磺酸钠的1％乙酸溶液-甲醇(74:26)为流动相;检测波长276 nm;流速:1.0 mL· min-1.结果:VB1在36.30～84.70 μg·mL-1;VB2在7.26～ 16.94 μg·mL-1;VB6在10.93～25.51μg·mL-1与烟酰胺在36.20～84.48 μg·mL -1的范围内峰面积与浓度具有良好线性关系;VB1,VB2,VB6与烟酰胺的回收率依次为:99.78％,RSD=1.58％(n=6);99.80％,RSD=1.22％ (n =6);100.07％,RSD=0.75％ (n=6);99.62％,RSD=1.01％ (n =6).结论:该方法准确,灵敏度高,重现性好.     

HPLC法测定五维B颗粒中四组份的含量

目的：建立一种高效液相色谱法测定五维B颗粒中烟酰胺、维生素B1、维生素B2、维生素B6的含量测定方法。方法：高效液相色谱法，ODS柱（4．6mm×250mm，5μm），流动相：甲醇-5mmol·L^-1庚烷磺酸钠（含0．5％冰醋酸＋0．1％三乙胺）（28：72），检测波长为280nln，流速1．0mL·min^-1。结果：烟酰胺、维生素B1、维生素B2、维生素B6的线性回归方程为：A烟酰胺=1．08×10^4C＋2．85×10^4，r=0．9997，n=3；A维生素B1=1．68×10^4C＋0．85×10^4，r=0．9999，n=3；A维生素B2=2．08×10^4C＋1．85×10^4，r=0．9999，n=3；A维生素B6=2．14×10^4C＋0．79×10^4，r=0．9999，n=3；线性范围分别为：105．25—526．25mg·L^-1；40．05—200．25mg·L^-1；21．35—106．75mg·L^-1；4．15—20．75mg·L^-1。结论：该方法准确，灵敏度高，重现性好，可作为质量检验的定量方法。