组学技术在食品安全检测中的应用

食品安全是全球关注的热点,食品安全检测是保障食品安全的重要环节。随着消费者对食品安全要求的提高,传统检测技术已经无法满足食品安全检测多样性的需求。近年来以基因组学、蛋白组学、代谢组学为代表的组学技术迅速发展,为食品安全检测带来了新突破。本文对近年来蛋白组学、代谢组学和基因组学技术在食品安全检测方面的应用进行了综述,并对未来组学技术应用于食品安全检测的发展趋势进行了展望。     

基于智能手机定量测定蛋白质的方法研究

利用智能手机完成了蛋白质浓度的检测,确定了用于图像比色的参数,方法适用于有颜色反应的分析物浓度检测。利用该法检测的相关系数大于0. 99,检出限为0. 21 g/L。考察了不同品牌手机的检测效果,结果表明,检测效果与手机硬件的配置无明显关联。考察了该方法的重复性,对单个样本检测时,3种质量浓度样本的相对标准偏差(RSD)分别为2. 0%、4. 6%、11. 9%;对4个样本进行同时检测,RSD分别为2. 2%、3. 8%、3. 5%、11. 5%。考察了亮度、色温、拍摄距离的影响,结果显示,亮度与色温对检测结果无影响,而拍摄距离有影响。手机APP与分光光度计对样本检测结果的相关系数(r2)为0. 969。该方法准确、重复性高、便携、操作方便,可实现多种分析物实时现场的快速检测。     

MOFs传感器在癌症及其生物标志物检测中的应用

癌症是世界上最致命的疾病之一,因此癌细胞的有效捕获和敏感检测对基础研究以及临床诊断和治疗都具有重要意义。基于金属有机骨架(MOFs)的催化活性和固有的发光性能等特点,MOFs已被成功地开发为传感平台实现对癌症及其标志物的检测。综述了基于MOFs的电化学、荧光、电化学发光、比色传感器在癌细胞及核酸、蛋白质等生物标志物检测中近3年的研究进展,从MOFs材料,检测物类型,检测方法、检测能力等方面进行了综述,并对各自的特点进行了讨论,对以后MOFs纳米材料在癌症检测中的应用进行了展望。     

检测大肠杆菌的免疫生物传感器研究进展

大肠杆菌是人体内常见的食源性致病菌,对其检测极为重要。免疫生物传感器技术作为目前研究较热的一种技术,在大肠杆菌的检测方面有不错的进展。本文综述了电化学、光学、压电等类型免疫传感器近十年的研究进展,从检测原理、抗体固定方式、修饰材料、检测能力等方面进行了综述,并对各自的优劣势进行了讨论,对免疫传感器的发展趋势进行了总结与展望。     

电化学分析方法检测重金属离子研究进展

重金属难以生物降解,对环境和人类生命健康造成了严重威胁,因此,重金属的检测和重金属污染的治理十分必要。近年来,电化学分析方法对重金属离子的检测具有灵敏度高,分析速度快,可同时对多种金属离子进行检测等优点,成为了重金属检测领域的研究热点。本文综述了常见电化学检测方法的检测原理和发展现状,通过引入线性范围、检出限和回收率等参数,分别对电位分析法、电位溶出法和伏安法的检测效果进行阐述,讨论了各种方法的优缺点,并指出以后的研究方向,以期为电化学传感器的应用提供基础。     

新污染物检测技术研究进展

检测分析技术是开展新污染物治理工作的基础,是精准识别新污染物的重要手段。本文对持久性有机污染物、内分泌干扰物、抗生素以及微塑料等四大类新污染物的检测方法进行了总结,并对检测分析方法进行了比较。提出了下一步做好新污染物检测工作要加强检测标准方法的顶层设计,开发高通量、效率高的检测方法,重视样品前处理技术的标准化研究和标准试剂的研发。     

碳点在抗生素分析检测中的应用

抗生素的过度使用对环境造成了极大破坏,对其进行监测控制刻不容缓。常用的分析检测技术,如高效液相色谱(HPLC)、气相色谱(GC)、高效液相色谱-串联质谱(HPLC-MS/MS)等具有高效快速、重现性好、可自动化操作等优点。但对环境样品中抗生素的检测存在样品前处理过程繁琐、检测灵敏度低、实验成本高等问题。结合现有的检测技术发展新型材料,对提高抗生素的检测灵敏度具有重要意义。碳点(CDs)是一种尺寸介于0~10 nm之间的新型纳米材料,具有小尺寸效应、优异的电学和光学性质、良好的生物相容性等优点,已被广泛应用于环境样品中抗生素的检测。该综述对近5年CDs与传感器、色谱分析技术结合检测抗生素的应用进行了总结,并对其发展前景进行了展望。该文总结了CDs与分子印迹传感器、适配体传感器、电化学发光传感器、荧光传感器及电化学传感器相结合,及其在抗生素检测中的应用;对涉及的比率型传感器、阵列传感器等先进分析方法进行了举例评述;对CDs作为色谱固定相分离抗生素进行了阐述。文献表明,CDs结合传感器检测抗生素可有效提高检测灵敏度,但对复杂环境样品中抗生素的检测还面临着构建高选择性传感器、开发新型材料及数据处理等方面的挑战;目前,CDs作为色谱固定相对抗生素的材料分离,仍处于初步研究阶段,分离机理尚不明确,有待进一步深入研究。总之,CDs在环境样品中抗生素的检测方面仍面临一系列问题,随着人们对CDs的深入研究以及各种分析检测技术的不断发展,CDs将会在抗生素等环境污染物的检测中发挥重要作用。     

基于拉曼光谱的细菌检测研究进展

细菌是一种与人类生命活动息息相关的微生物, 其快速、 高灵敏检测对重大传染性疾病的防控至关重要. 本文介绍了拉曼光谱用于细菌检测的基本原理, 综述了3种拉曼光谱用于细菌检测的主要方式, 包括细菌组成成分检测、 细菌代谢物检测以及基于拉曼探针标记的检测模式, 并对各种拉曼检测方法进行了分析比较. 最后, 展望了拉曼光谱在细菌检测领域的发展前景, 并提出了5条建议.     

表面增强拉曼光谱在偶氮染料检测中的研究进展

简述了偶氮染料的检测现状,对偶氮染料研究中表面增强拉曼光谱检测方法进行了综述。介绍了表面增强拉曼光谱用金属溶胶、金属电极、金属薄膜3种增强基底在偶氮染料检测中的方向,并对其在偶氮染料检测中的研究前景进行了展望。表面增强拉曼光谱法是一种新型光谱分析技术,具有操作简单、快速、灵敏度高等优势,为偶氮染料的检测开辟了新道路。     

高效液相色谱法测定三聚氰胺的不确定度评定

分析了高效液相色谱法测定饲料中三聚氰胺的不确定度来源,并对各不确定度分量进行了评定,得出了三聚氰胺检测结果的相对合成标准不确定度。结果表明检测过程的精密度、检测程序的偏差及校准曲线对检测结果的不确定度影响最大。     

Separation and Determination of Cold Medicine Ingredients by Capillary Zone Electrophoresis Using Sulfated β‐Cyclodextrin as an Electrolyte Modifier and Chiral Selector

Capillary zone electrophoretic separations of cold medicine ingredients, including acetaminophen (AC), dextromethorphan (DMF) and racemates of phenylpropanolamine (PPA) and chlorpheniramine maleate (CPM) using randomly sulfated‐β‐CD (S‐β‐CD) as an electrolyte modifier and a chiral selector were investigated. The results indicate that S‐β‐CD is an excellent chiral selector and a suitable electrolyte modifier as well for the separation of those cold medicine ingredients. Influences of S‐β‐CD concentration and buffer concentration on the separation were examined. Baseline separation of these cold medicine ingredients with 1.0 % (w/v) S‐β‐CD could be simultaneously and successfully achieved within 11.8 minutes. In addition, S‐β‐CD could also act as a chiral selector for enantioseparation of PPA and CPM. A high enantioselectivity was obtained for these two analytes. Linear relationships between the peak area and its concentration for the calibration curves of AC and DMF were obtained (correlation coefficients: 0.9987 for AC, 0.9965 for DMF, respectively). The relative standard deviations of the migration time and peak area of AC and DMF were 0.19, 2.44 % and 0.34, 2.99 %, respectively. Detection limits were 0.93 and 2.57 μg/mL for AC and DMF, respectively. Recoveries of AC and DMF ranging between 102.42 and 97.28 % were observed. The proposed method was successfully applied to the determination of AC and DMF in cold medicines.     

在线扫集-胶束毛细管电动色谱法测定复方氨酚烷胺胶囊中的3种有效成分

以在线扫集-胶束毛细管电动色谱法(Sweeping-MEKC)测定了复方氨酚烷胺胶囊中的马来酸氯苯那敏、咖啡因和对乙酰氨基酚3种有效成分。考察了缓冲溶液pH值、SDS浓度、分离电压及进样时间等对分离效果的影响。优化条件:以未涂层熔融石英毛细管(55 cm×50μm,有效柱长35 cm)为分离柱;环境温度25℃;80 mmol/L十二烷基磺酸钠+20 mmol/L NaH2PO4(pH 2.2)+15%乙腈为缓冲体系,分离电压-20kV,进样时间60 s(H=20.0 cm),测量波长210 nm。在该条件下氯苯那敏、咖啡因和对乙酰氨基酚在25min内出峰,峰面积RSD均小于4%;线性范围分别为2.45～39.17、1.61～25.76、1.58～25.28 mg/L;检出限(S/N=3)分别达139、34、24μg/L,回收率分别为96%～101%、98%～102%、96%～102%。     

Simultaneous determination of some active ingredients in cough and cold preparations by gas chromatography, and method validation

A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 microL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m x 0.22 mm; film thickness, 0.25 microm). The column temperature was held at 150 degrees C for 5 min, increased to 175 degrees C at 3 degrees C/min, and increased to 270 degreesC at 10 degrees C/min. The temperatures of the flame ionization detector and injector were maintained at 300 degrees C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies.     

高效液相色谱双波长检测法测定维C银翘片中4种组分的含量

建立了高效液相色谱测定维C银翘片中维生素C、对乙酰氨基酚、马来酸氯苯那敏和绿原酸4种组分含量的方法。研究优化了样品提取的溶剂与超声提取条件、色谱分离条件和检测波长等,采用了Sinochrom ODS-BP(4.6 mm×200 mm, 5 μm)色谱柱,以0.05 mol/L KH2PO4(pH 3.0,含1%三乙胺)-乙腈(75:25, v/v)为流动相,双检测波长260 nm和326 nm等分离检测条件。结果表明,维生素C、对乙酰氨基酚、马来酸氯苯那敏和绿原酸的测定线性范围均比较宽,方法平均回收率大于99.4%,相对标准偏差(RSD)小于1.8%(n=5),而且测定方法快速、简便、准确,非常适合维C银翘片类药物的质量控制。     

Application of experimental design in optimization of the separation condition for determination of four active components in cold medicines by flow injection-capillary electrophoresis

Orthogonal design (OD) was employed to optimize the separation condition of flow injection-capillary electrophoresis (FI-CE). In order to compare the optimum condition, uniform design and univariate approach were also adopted. The influences of variables such as buffer pH, buffer concentration, acetonitrile (ACN) percentage, and separation voltage were discussed. The optimum separation condition was established. The limits of detection were 1.94 × 10(-2), 6.40 × 10(-3), 1.16 × 10(-2) and 1.94 × 10(-2) μg/mL for dextromethorphan hydrobromide (Dex), chlorphenamine hydrogen maleate (Chl), pseudoephedrine hydrochloride (Pse), and paracetamol (Par), respectively. The RSDs of peaks areas were less than 2.0%. The results showed the OD was an effective method among experimental designs for optimizing the separation conditions of CE. The optimum condition was used for separation and determination of Dex, Chl, Pse, and Par in cold medicines. The average recovery was between 96.68-101.25%.     

Structure analysis of aromatic medicines containing nitrogen using near-infrared spectroscopy and generalized two-dimensional correlation spectroscopy

Four aromatic medicines (acetaminophen; niacinamide; p-aminophenol; nicotinic acid) containing nitrogen were investigated by FT-NIR (Fourier transform near-infrared) spectroscopy and generalized two-dimensional (2D) correlation spectroscopy. The FT-NIR spectra were measured over a temperature range of 30-130 degrees C. By combining near-infrared spectroscopy, generalized 2D correlation spectroscopy and references, the molecular structures (especially the hydrogen bond related with nitrogen) were analyzed and the NIR band assignments were performed. The results will be helpful to the understanding of aromatic medicines containing nitrogen and the utility of these substances.     

Simultaneous Determination of Dextromethorphan Hydrobromide, Pyrilamine Maleate and Sodium Benzoate in a Cough Cold Syrup by LC

A liquid chromatographic method for the simultaneous determination of dextromethorphan hydrobromide, pyrilamine maleate and sodium benzoate in cough cold syrup has been developed. The method was based on replacing heptane sulfonate by sodium chloride as ion pairing agent. The addition of sodium chloride to the mobile phase has changed the retention behaviour of the basic drugs. The separation of these compounds was achieved in less than 8 min with an isocratic mobile phase consisting of acetonitrile/0.1 M dihydrogenphosphate buffer containing 0.1 M sodium chloride (29:71 v/v) at pH 2.5 and using a Kromasil C18 column. The analysis was performed at a flow rate of 1 mL min^?1 and at a detection wavelength of 220 nm. The selectivity, linearity of calibration, accuracy, within and between days precision, limit of detection and quantification, recovery were examined as parts of the method validation. Calibration curves were linear in the range 1–140 μg mL^?1 with a regression coefficient (R ²) better than 0.999. The results of the method repeatability (intra-day) and reproducibility (inter-day) were all less than 2% (n = 6). The lowest detectable concentration of dextromethorphan hydrobromide and pyrilamine maleate varied between 0.10 and 0.12 μg mL^?1. The proposed liquid chromatographic method was satisfactorily applied for the routine quality control of dextromethorphan hydrobromide, pyrilamine maleate and sodium benzoate in cough cold syrup formulations.     

Simple HPLC method for simultaneous determination of acetaminophen, caffeine and chlorpheniramine maleate in tablet formulations

Summary A simple, rapid and accurate, routine-HPLC method is described for simultaneous determination of acetaminophen, caffeine and chlorpheniramine maleate in a new tablet formulation Chromatographic separation of the three pharmaceuticals was achieved on a Hypersil CN column (150×5.0 mm, 5 μm) using a mobile phase comprising a mixture of acetonitrile, an ion-pair solution and tetrahydrofuran (13:14:87, v/v,pH4.5). The flow-rate was changed from 1.0 mL min⁻¹ (in 0≈7.5 min) to 1.8 mL min⁻¹ (after 3.5 min). was complete in <10 min. The method was validated for system suitability, linearity, accuracy, precision, limits of detection and quantitation, and robustness. Linearity, accuracy and precision were found to be acceptable over the ranges 31.6≈315.8 μg mL⁻¹ for acetaminophen, 9.5≈94.6 μg mL⁻¹ for caffeine and 1.4≈13.8 μg mL⁻¹ for chlorpheniramine maleate.     

Simultaneous Determination of Acetaminophen, Caffeine, and Chlorphenamine Maleate in Paracetamol and Chlorphenamine Maleate Granules

A simple and rapid HPLC method using phenacetin (PHN) as internal standard has been developed for simultaneous determination of acetaminophen, caffeine, and chlorphenamine maleate in the product compound paracetamol and chlorphenamine maleate granules. Separation and quantitation were achieved on a 250 mm × 4.6 mm, 5 μm particle, C₁₈ column. The mobile phase was methanol 0.05 mol L^?1 aqueous KH₂PO₄ solution, 45:55 (v/v), containing 0.1% triethylamine and adjusted to pH 3.6 by addition of phosphoric acid; the flow rate was 1.0 mL min^?1. Detection of all compounds was by UV absorbance at 260 nm and elution of the analytes was achieved in less than 12 min. The linearity, accuracy, and precision of the method were acceptable to good over the concentration ranges 6.4–153.6 μg mL^?1 for acetaminophen, 5.0–120.0 μg mL^?1 for caffeine, and 9.6–230.4 μg mL^?1 for chlorphenamine maleate.     

Simultaneous Quantitative Determination of Codeine Phosphate,Chlorpheniramine Maleate Phenylephrine Hydrochloride and Acetaminophen in Pharmaceutical Dosage Forms Using Thin Layer Chromatography Densitometry

Abstract

A simple and specific method for the analysis of codeine phosphate, chlorpheniramine maleate, phenylephrine hydrochloride and acetaminophen in pharmaceutical dosage forms was developed. The procedure consists of direct application of diluted liquid dosage forms and the solutions of solid dosage forms on silica gel plates. The mobile phase for development consisted of n-butanol-methanol-toluene-water and acetic acid. The separated components were measured quantitatively by densitometry. Linearity, reproducibility and percentage recovery of active ingredients from dosage forms were calculated.