HPLC法对三种食品添加剂的应用

本文旨在建立一种快速测定食品中苯甲酸、山梨酸、糖精钠的高效液相色谱法。本方法以YWG—C18柱,甲醇：乙酸铵为流动相,研究其三种物质的色谱分离特性,并对食品样品的前处理方法进行探讨。经实践得到了快速、有效的分离和样品处理方法。该方法测定的三种物质浓度在0—0．100mg／ml之间呈线性关系,相关系数在0．999以上,证明该法准确度高、重现性好。应用于多种食品样品的测定,结果令人满意。     

高效液相色谱法测定CO2膨胀前后烟丝中氨基酸

本文研究了用Waters柱前衍生试剂AQC,即6-氨基喹啉基-N-羟基琥珀酰亚氨基酸甲酸来测定CO2膨胀前后烟丝中的氨基酸的组成和含量,流动相由磷酸盐缓冲液、乙腈和纯水构成,梯度洗脱。结果表明:烟丝在CO2膨胀前后样品所测16种游离氨基酸的总量普遍减少。     

Development and validation of a rapid HPLC method for the determination of ketotifen in pharmaceuticals

In the present study, a simple, sensitive, rapid, and stability-indicating high performance liquid chromatographic (HPLC) method with ultraviolet detection for the analysis of ketotifen was developed and validated. The method was applied to the determination of ketotifen in pharmaceutical formulations (tablets and syrups). The HPLC method utilized isocratic elution technique with a reversed phase C8 column, detection at 297 nm and a mixture of methanol, triethylamine phosphate buffer (pH 2.8; 0.04 M), and tetrahydrofuran (43: 55: 2, v/v/v) as mobile phase at a flow rate of 1.2 mL/min. Total analysis time was about 7 min with typical retention time of ketotifen of about 5 min. The method was validated for selectivity, linearity, accuracy, and precision following International Conference of Harmonization, 1996 (ICH) recommendations. Due to its simplicity and accuracy, the method can be used for routine quality control analysis.     

高效液相色谱法测定面粉中增白剂加入量

本文提出高效液相色谱法测定面粉中增白剂过氧化苯甲酰(BPO)及其还原产物苯甲酸(BA)的新方法。用乙醇为溶剂通过超声波提取面粉中的过氧化苯甲酰及其还原产物,用HPLC可同时测定BPO和BA含量;该方法具有良好的分离度、准确性和再现性。     

Simultaneous determination of methocarbamol and aspirin in presence of their pharmacopeial-related substances in combined tablets using novel HPLC-DAD method

Objective and Significance: Methocarbamol (MET) and aspirin (ASP) are widely used as a muscle relaxant combination. The USP reports guaifenesin (GUA) and salicylic acid (SAL) as related substances and hydrolytic products of MET and ASP, respectively. This work aimed at developing and validating a simple and sensitive RP-HPLC method for the determination of both drugs as well as their related substances (at their pharmacopeial limits) in their bulk powders, laboratory prepared mixtures, and MET-ASP combined tablets. Methods and Results: Chromatographic separation was achieved in less than 9?min with the required resolution, peak symmetry, and accuracy on C₁₈ column using isocratic elution system of diluted acetic acid (pH 3.2): acetonitrile at the ratio of 79: 21, v/v, at a flow rate of 1?mL/min. Detection was achieved with photodiode array at 233?nm for MET, GUA, and SAL and at 273?nm for ASP. The developed method has been validated as per ICH guidelines and the calibration plots were linear over the concentration ranges of 2–150, 0.4–30, 25–450, and 0.2–27?μg/mL for MET, GUA, ASP, and SAL, respectively. Conclusion: The optimized method proved to be specific, robust and precise for the quality control of the studied drugs in pharmaceutical preparations to ascertain that their related substances are not exceeding the permitted pharmacopeial limits.     

固相萃取-高效液相色谱法测定水中邻苯二甲酸酯类的方法研究

建立了固相萃取-高效液相色谱法测定水中5种邻苯二甲酸酯类的方法。通过正交实验确定了固相萃取的最优化条件：洗脱剂组成（乙醚：甲醇）19：1,洗脱速率1．0mL／min,洗脱体积9mL,清洗剂组成（甲醇：水）1：19。液相色谱的最佳条件：检测波长224nm,流速1．0mL／min,采用梯度洗脱,开始时甲醇-水（75：26,V／V）,保持6min,第7min甲醇比例上升到100％。结果,5种物质峰面积对浓度进行线性回归的相关系数均大于0．9992,该方法的最低检出限在（0．01～0．07）pg／L之间,加标回收率82．1％～97．4％,相对标准偏差（RSD）1．1％～2．4％。     

固相萃取-液相色谱法测定糕点中脱氢乙酸、苯甲酸、山梨酸的方法研究

建立了固相萃取-高效液相色谱法测定糕点中的脱氢乙酸、苯甲酸、山梨酸的方法。实验结果表明,在(0.02～0.15)mg/mL时有良好的线性关系(r>0.997),相对标准偏差(RSD)为1.0%～2.5%,回收率96.2%～102.1%。该方法简单、快速、灵敏度高,并具有良好的精密度与准确度,可作为糕点中检测防腐剂的有效定量方法。     

藏药牦牛血粉饮片中氨基酸和无机元素测定

为建立藏药牦牛血粉饮片中氨基酸和无机元素的定性和定量分析方法,试验采用高效液相色谱-柱后衍生法对牦牛血粉中游离氨基酸进行测定:离子交换柱(2.5 mm×150 mm,6μm),检测波长为570 nm、440 nm,测试方法为单点矫正法;采用微波消解-ICP-MS对牦牛血粉中无机元素进行测定:测定模式为碰撞反应模式,碰撞气(He)流量5 mL/min。数据采集模式:跳峰扫描,采样深度8.0 mm,重复扫描3次。结果表明:牦牛血粉中含有一定量的游离氨基酸,其中包括8种人体必须氨基酸。无机元素以Al、Na、Mg、K、Ca、Fe为主,还含有V、Cr、Mn、Zn、Co、Ni、Cu、Se等人体所需微量元素,各无机元素均在浓度考察范围内,线性关系良好(r^2>0.9984),加样回收率在99.2%~108.4%之间。该研究初步明确藏药牦牛血粉饮片中氨基酸和无机元素的组成,方法准确高效,为综合评价藏药牦牛血粉饮片的质量提供科学依据和方法参考。     

Multivariate analysis of anionic, cationic and nonionic textile surfactant degradation with the H(2)O(2)/UV-C process by using the capabilities of response surface methodology

Anionic, cationic and nonionic surfactants being frequently employed in the textile preparation process were subjected to H(2)O(2)/UV-C treatment. As a consequence of the considerable number of parameters affecting the H(2)O(2)/UV-C process, an experimental design methodology was used to mathematically describe and optimize the single and combined influences of the critical process variables treatment time, initial H(2)O(2)concentration and chemical oxygen demand (COD) on parent pollutant (surfactant) as well as organic carbon (COD and total organic carbon (TOC)) removal efficiencies. Multivariate analysis was based on two different photochemical treatment targets; (i) full oxidation/complete treatment of the surfactants or, alternatively, (ii) partial oxidation/pretreatment of the surfactants to comply with the legislative discharge requirements. According to the established polynomial regression models, the process independent variables "treatment time" (exerting a positive effect) and "initial COD content" (exerting a negative effect) played more significant roles in surfactant photodegradation than the process variable "initial H(2)O(2) concentration" under the studied experimental conditions.     

Investigation of the molecular state of 4-aminosalicylic acid in matrix formulations for dry powder inhalers using solid-state fluorescence spectroscopy of 4-dimethylaminobenzonitrile

Carrier-free method is an alternative approach for dry powder inhaler (DPI) formulations, which overcome poor drug mobility and distribution. Here we investigated the properties of an active pharmaceutical ingredient (API) within composite particles. We used highly-branched cyclic dextrin (HBCD) as the excipient matrix that was prepared using a spray-drying technique. 4-Aminosalicylic acid (4-ASA) and 4-dimethylaminobenzonitrile (DMABN) were selected as a hydrophilic second-line antitubercular agent and a surrogate for 4-ASA as a model compound, respectively. The spray-dried particles (SDPs) containing 4-ASA or DMABN with HBCD had geometric median diameters (D₅₀) of 2.34 ± 0.07 μm and 2.26 ± 0.10 μm, respectively. Further, the in vitro aerodynamic properties were similar for SDPs containing 4-ASA and DMABN with HBCD. To determine the properties of APIs within composite particles, we performed solid-state fluorescence spectroscopy of DMABN. As a candidate excipient, hydroxypropyl methylcellulose (HPMC) was compared to HBCD. We determined the intensity ratio of twisted intramolecular charge transfer (TICT) emission to locally excited emission within the excipient matrix environment. The HBCD matrix environment was better than HPMC to trigger a more robust TICT reaction of DMABN. A potent state-changing interaction of APIs occurred in the HBCD matrix environment versus another excipient environment.