Determination of Curcuminoids and Their Degradation Products in Turmeric (<Emphasis Type="Italic">Curcuma longa</Emphasis>) Rhizome Herbal Products by Non-aqueous Capillary Electrophoresis with Photodiode Array Detection

Non-aqueous capillary electrophoresis (NACE) method was optimised for simultaneous determination of major bioactive curcuminoids (CCD) viz., curcumin (CC), desmethoxycurcumin (DC) and bisdesmethoxycurcumin (BC), and some of the degradation products viz., vanillin (VN), vanillic acid (VA), ferulic acid (FA) and 4-hydroxybenzaldehyde (HB) in turmeric milk and herbal products. Separation was achieved using non-aqueous background electrolyte (NA-BGE), consisting of a mixture of sodium tetraborate, sodium hydroxide, methanol and 1-propanol in a single run by capillary electrophoresis (CE). In the present study, a novel ultrasonication-assisted phase separation method (US-PS) was used for extracting the analytes in turmeric milk and the extract was directly injected into the capillary without any pretreatment. High-performance thin layer chromatographic (HPTLC) method for the separation of the analytes was also evaluated on pre-coated silica gel plate. Two different high-performance liquid chromatographic (HPLC) conditions were reported in the literature for the separation of above-mentioned target compounds. The proposed method NACE is simple, fast, convenient and economical.     

加压毛细管电色谱法分离检测薯片中丙烯酰胺的含量

建立加压毛细管电色谱法检测薯片中丙烯酰胺含量的方法。该方法采用EP-100-20/45-3-C18毛细管色谱柱（总长度45?cm,有效长度20?cm,直径100?μm,ODS填料3?μm）进行分离,并对流动相中有机相比例、磷酸盐缓冲溶液浓度、分离电压等实验条件进行考察和优化。结果表明：在流动相为乙腈-15?mmol/L?NaH2PO4（pH?4.7）缓冲盐溶液（15∶85,V/V）,流动相流速为0.04?mL/min,分离电压为－2?kV,紫外检测波长为202?nm的条件下,薯片中的丙烯酰胺得到了良好地分离。方法在2.0～32?μg/mL范围内线性关系良好,相关系数为0.999?4。丙烯酰胺检出限（RSN=3）为0.30?μg/mL,平均回收率为95.3%～108.1%,相对标准偏差低于1.48%。该方法已经用于薯片中丙烯酰胺含量测定,结果良好。     

Detection of GM Canola MS11, DP-073496-4, and MON88302 events using multiplex PCR coupled with capillary electrophoresis

As of 2020, 11 GM canola events have been authorized as food for humans in Korea. However, there are no simultaneous multiplex detection methods for 3 GM canola events (DP-073496-4, MON88302, and MS11). Thus, we established the multiplex polymerase chain reaction (PCR) method coupled with capillary electrophoresis to detect 3 GM canola events. To verify the specificity of event-specific primers, various GM crops of 3 GM soybean events, 6 GM maize events, 2 GM cotton events and 11 GM canola events were prepared. The limit of detection of the developed multiplex PCR was approximately 0.0125% for 3 GM canola events. Certified GM canola and stacked events were analyzed to validate the developed multiplex PCR. This study focuses on establishing multiplex PCR coupled with capillary electrophoresis for newly approved GM canola events and contributes to efficient monitoring GM canola samples in Korea.     

高效毛细管区带电泳法同时检测3个产地沙棘果粉中的活性物质

利用高效毛细管区带电泳法,对3个产地沙棘果粉中的芦丁、山柰酚、异鼠李素、槲皮素4种活性物质进行同时分离测定。考察不同电泳条件对分离效率的影响,得出最佳电泳条件:缓冲溶液20 mmol/L Na_2B_4O_7-H_3BO_3(质量浓度为1.5 mg/mL的β-环糊精),pH 9.55,检测波长370 nm,分离电压25 kV,进样时间5 s。在该条件下,芦丁、山柰酚、异鼠李素、槲皮素4种活性物质在11 min内得到分离,线性范围分别为0.01~0.51、0.05~0.93、0.02~0.65、0.03~0.81 mg/mL,相关系数在0.997 1~0.999 1之间,检出限分别为5.05×10~(-5)、2.10×10~(-5)、3.75×10~(-5)、1.31×10~(-5) mg/mL(RSN=3),各物质线性关系良好。日内及日间精密度范围为0.08%~4.72%,平均回收率在95.51%~104.66%之间,相对标准偏差不大于3.92%(n=3)。在优化条件下,对4种活性物质标准品的混合物进行测定,并用相同方法对3个产地沙棘果粉中活性物质的提取液进行检测。结果表明:不同产地沙棘中,4种被检测化合物的含量各不相同。沙棘中被测4种化合物总量最高的产自新疆乌鲁木齐,最低的产自甘肃武威,而槲皮素含量以产自山西吕梁的最高,山柰酚和异鼠李素以产自新疆乌鲁木齐最高。本方法快速简便、准确可靠,可用于沙棘果粉中多种活性物质的同时检测。     

毛细管电泳法同时分离检测饮料中的六种食品添加剂

建立毛细管电泳法同时测定饮料中苯丙氨酸、对羟基苯甲酸甲酯、肉桂酸、山梨酸钾、抗坏血酸和苯甲酸6种食品添加剂的分析方法。在Peakmaster 5.3软件对电泳参数模拟的基础上,考察了缓冲液浓度、pH值以及分离电压对6种食品添加剂分离效果的影响。结果表明,在检测波长214 nm,进样时间10 s的情况下,确定最佳电泳条件为40 mmol/L pH 9.0 Na2HPO4-H3PO4的缓冲液,分离电压12 kV。在此条件下,6种食品添加剂在20～160 mg/L范围内呈良好的线性关系（R＞0.980 0）,检出限为0.23～0.77 mg/L,加标回收率为97.3%～103.0%,相对标准偏差（RSD）为2.0%～3.8%,精密度试验结果相对标准偏差（RSD）为2.0%～3.8%,表明该方法操作简便、准确度高、精密度良好,能满足饮料中6种食品添加剂的检测需求。     

Simultaneous Determination of Acephate and Isocarbophos in Vegetables by Capillary Electrophoresis Using Ionic Liquid and Sodium Dodecyl Sulfate as Modifiers

In this study, an improved method of capillary electrophoresis for simultaneous detection of acephate and isocarbophos was developed. The ionic liquids (ILs) of 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF₄) and sodium dodecyl sulfate (SDS) were added as modifiers in the background electrolyte (BGE) for capillary electrophoresis to enhance the separation efficiency of acephate and isocarbophos. The separation conditions in terms of the concentrations of the IL, SDS, and pH were optimized. The limits of detection of the method for acephate and isocarbophos were 0.15 and 0.08 mg/kg. The relative standard deviation (RSD) for five replicates of acephate and isocarbophos solution (5.0 mg/L) was 1.9–3.9%, respectively. To evaluate the accuracy of this method, cucumber, cauliflower, spinach, and carrot samples spiked with acephate and isocarbophos were extracted and analyzed with good recoveries from 76.8 to 88.8%. This method was then verified by gas chromatography method.     

Development of a modular system for detection of genetically modified organisms in food based on ligation-dependent probe amplification

The application of a method based on ligation-dependent probe amplification to the simultaneous detection of different genetically modified organisms in food is described. The ligation reaction of target-specific probes with characteristic lengths and universal primer binding sites is followed by PCR amplification using fluorescein-labeled primers. The separation and the detection of DNA fragments are achieved by capillary electrophoresis via laser-induced fluorescence. The approach allows the simultaneous detection of several targets corresponding to different levels of specificity in a one-tube assay. Synthetic oligonucleotides were designed to detect (1) reference genes in the genome from maize, soya and rapeseed, (2) the CaMV 35S-promotor as screening element, (3) the construct-specific 35S-pat junction, and (4) the event-specific regions of the transgenic maize line MON 810 and of Roundup Ready soya. Specificity and sensitivity (GMO content 0.1%) of the approach were shown for all targets. This novel analytical strategy represents a flexible, modular system for the surveillance of GMO-derived products that can be readily complemented by further target sequences of interest.     

基于涂层法的凝胶复合型智能抗浸面料制备

为开发新型智能抗浸面料,采用涂层方法使温敏性共聚物聚（N-叔丁基丙烯酰胺-co-丙烯酰胺）（简称P(NTBA-co-AAm)）通过交联剂BTCA的作用转变成三维交联凝胶,并使凝胶与棉织物结合。通过红外光谱法及环境扫描电镜观察证明,涂层织物表面确实结合上了P(NTBA-co-AAm)交联凝胶,对涂层织物的温度敏感性、阻水性、透湿性进行探讨。结果表明,棉织物与凝胶结合后,阻水性能大大增强,当增重率增大到一定程度后可以做到完全阻水,而且在水中时对温度变化也有响应,但透湿性有所下降。得到的温敏性凝胶复合型织物能满足抗浸面料的基本要求,可以进一步研究开发。     

Fast determination of N-phenylpropenoyl-l-amino acids (NPA) in cocoa samples from different origins by ultra-performance liquid chromatography and capillary electrophoresis

N-Phenylpropenoyl-l-amino acids (NPA) are among the key contributors to the astringent taste of cocoa. Two fast and easy to use methods (CE and UPLC?, both with PDA detection) for routine determination of the main NPA were developed. Crude extracts of defatted seeds were analysed by means of capillary electrophoresis leading to separation in less than 30min. Separation by means of UPLC? was much faster (<4min), however, a preceding SPE clean-up abolishes this benefit in time saving. Thus, the CE- and UPLC?-methods are comparable concerning time consumption and provide similar results. Analysis of 18 samples of raw and roasted beans from the global cocoa market originated from 12 countries and 4 continents showed a great variability of NPA content (0.7-3.6mg/g) and qualitative composition of different NPA. Anyway, all samples from cocoa beans showed a comparable NPA pattern. N-[3',4'-dihydroxy-(E)-cinnamoyl]-l-aspartic acid was the most abundant metabolite, followed by N-[4'-hydroxy-(E)-cinnamoyl]-l-aspartic acid and N-[3',4'-dihydroxy-(E)-cinnamoyl]-3-hydroxy-l-tyrosine (clovamide). The analysis of other plant organs (flowers, leaves, fruits) revealed an entirely different situation. NPA were detected in all parts of the fruit, with husk and pulp being clearly dominated by clovamide. In flowers and leaves no NPA were detected; 2-O-caffeoyltartaric acid was shown to be the major caffeic acid metabolite in leaves.     

电泳法在食品过敏原检测中的应用

本文简要介绍了食品过敏原的检测特点和难点,比较了目前常用的聚合酶链式反应法、环介导等温扩增法、酶联免疫法、液相色谱法和液相色谱质谱法等检测方法的优劣势。主要介绍了电泳技术的特点,总结了经典电泳技术在食品过敏原分析上的应用现状。详细介绍了近年来毛细管电泳技术在食品过敏原检测研究方面取得的进展,列举了区带毛细管电泳法、亲和毛细管电泳法、凝胶毛细管电泳法、动态涂层毛细管电泳法和芯片毛细管电泳法在致敏蛋白分析方面的应用,并对电泳法在食品过敏原分析中的发展趋势进行了展望。     

毛细管电泳-电化学发光分离检测辣椒粉中罗丹明B

建立一种以三联吡啶钌（Ru(bpy)32＋）为发光体系的毛细管电泳-电化学发光检测系统,并将其应用于分离和测定辣椒粉中的罗丹明B含量。考察检测电压、Ru(bpy)32＋溶液浓度、磷酸盐缓冲液的pH值和浓度、分离电压、进样电压与进样时间等因素对分离检测的影响。结果表明：在检测电压1.14 V、Ru(bpy)32＋溶液浓度5 mmol/L、磷酸盐缓冲溶液浓度20 mmol/L（pH 8.0）、进样时间10 s、进样电压10 kV、分离电压15 kV条件下,罗丹明B在6 min中得到分离。方法的线性范围为5×10－7～5×10－5 mol/L,检出限为1×10－7 mol/L（RSN=3）。对1.0×10－5 mol/L的罗丹明B标准溶液连续测定5 次,迁移时间和峰面积的相对标准偏差分别为3.2%和1.5%。该方法可成功应用于辣椒粉中罗丹明B含量的测定。     

3种毛细管电泳方法分析牛乳蛋白的比较

对比毛细管凝胶电泳(CGE)、毛细管未涂层管区带电泳(CZE)和涂层管区带电泳(CZE)在牛乳蛋白分离和定量分析,结果表明在分离条件、分离效果和定量特征上,毛细管涂层区带电泳优于其他两种电泳。应用涂层毛细管区带电泳对不同阶段婴幼儿配方乳粉的蛋白组成进行测定,分离效果较好。     

毛细管电泳法分离检测香兰素、香兰素醇、香兰素酸和阿魏酸

建立同时测定香兰素、香兰素醇、香兰素酸和阿魏酸4种组分的毛细管电泳法。研究运行缓冲液的组成、pH值和浓度、分离电压、进样时间及检测波长等对分离效率的影响,获得最优的测定条件。以熔融石英毛细管为分离通道,工作电极电位20kV、20℃、进样时间5s、检测波长280nm,在pH9.23、浓度30mmol/L硼砂缓冲液中,4组分获得良好的分离。该法应用于当归、胡黄连和奶糖等样品的检测分析,结果令人满意。     

MAJOR VOLATILES IN TOASTED CANOLA OIL

Headspace volatiles from 'Alto' canola oil toasted at 240C for 8 min were collected using Tenax ^R TA 60/80 (Supelco Inc., Bellefonte, PA). The Tenax ^R was washed three times with a total of 6 ml of solvent. The solvent extract was concentrated by drying in a hood at room temperature for 6 h. Two μl of concentrated extract were separated on a 30 m DB-1 capillary column (J & W Scientific, Folson, CA) with a Hewlett Packard (HP) 5890A gas chromatograph connected to a HP 5790 mass spectrometer. Volatiles were tentatively identified with a NBS 43 K.1 library by PBM (probability based on matching) search.
Fifty seven peaks were detected by the mass spectrometer. Among those, 50 compounds were tentatively identified. 2-Furancarboxaldehyde, 5-methyl-2-furan carboxaldehyde, 5-(1-methyl ethyl)-1,3-cyclopentadiene, cyclododecane, undecanoic acid, tetradecanoic acid, 1-hexadecanol, hexadecanoic acid, 9-octadecenoic acid, octadecanoic acid, 2,5-dimethyl pyrazine, 3-ethyl-2,5-dimethyl pyrazine, [1,1':3',1"-terphenyl]-1'-ol and [1,1':3',1"-terphenyl]-4'-ol were the major volatile compounds.     

大豆多肽分离纯化技术研究进展

文章介绍了多种大豆多肽分离纯化技术如膜分离(超滤、纳滤、微滤),色谱(正交轴逆流色谱、反相高效液相色谱,凝胶过滤色谱,离子交换色谱),毛细管电泳(毛细管区带电泳、胶束电动毛细管电泳、毛细管凝脉电泳)以及联用技术,分析了这些技术的基本原理及各自的优点,并对大豆多肽分离纯化的最新研究进展进行了综述。     

两种快速分离检测南方水牛乳乳清蛋白方法的比较

采用了毛细管电泳法(CE)和反相高效液相色谱法(RP-HPLC)两种方法对乳源乳清蛋白进行分离检测。结果表明:两种方法都能够有效分离乳清蛋白中的BSA,α-La,β-Lg,并能对各种蛋白进行定性定量分析。相比而言,毛细管电泳法分离更加快速,整个分离过程7 min左右即可完成,能分离出IgG组分。而RP-HPLC分离时间更长,需要45 min才能完全分离,并且无法分离出IgG组分。     

等离子体引发亚麻接枝改性方法的优化设计

研究了低温等离子体引发亚麻接枝丙烯酰胺(AAm)的优化设计方法,以改善其染色性能。采用二次回归正交设计法建立亚麻织物上染率与接枝液浓度、温度、等离子体处理电压、时间之间的函数表达式,并分别列出每种因素单独的函数表达式。最终确定最优工艺为接枝液质量分数30%,温度25℃,电压14.6 kV,时间60 s。     

Detection method for genetically modified papaya using duplex PCR

A simple and rapid method for the identification of genetically modified (GM) papaya, derived from Line 55-1, was developed by modifying the Japanese official PCR method. Genomic DNA was directly extracted from the fresh fruit without the lyophilization step, using a commercial silica-based kit. To develop a duplex PCR method which simultaneously detects the GM papaya-specific gene and the intrinsic papain gene, the papain 2-5'/3' (amplicon size; 184 bp) primer pair for the detection of the papain gene was newly designed within the region of the products (211 bp) amplified using the papain 1-5'/-3' primer pair adopted in the Japanese official PCR method. To detect the GM papaya-specific gene, the primer pair Nos C-5'/CaM N-3' described in the Japanese official method was used. The DNA sequences of the GM papaya gene and the intrinsic papain gene were co-amplified using the PCR method in a single tube. The developed duplex PCR method allows the simultaneous detection of the products by means of agarose gel electrophoresis or microchip electrophoresis. The proposed method for GM papaya identification is simple and rapid.     

高效毛细管电泳法测定酱油中5'-单磷酸核苷酸

建立高效毛细管电泳同时分离测定酱油中两种核苷酸鸟嘌呤-5O`-单磷酸(GMP)和次黄嘌呤-5O`-单磷酸(IMP)的方法。电泳条件：以50μm×60.2cm(有效长度50cm)未涂敷石英毛细管为分离柱,30mmol/L硼砂＋30mmol/L碳酸钠＋60mmol/L羟丙基-β-环糊精为分离缓冲溶液,50mmol/L醋酸溶液为样品介质,检测波长为254nm。GMP及IMP的校正峰面积与质量浓度在5～100mg/L范围内具有良好线性关系,线性相关系数分别为0.9998和0.9997,检出限均为2mg/L,定量限均为5mg/L。用该法测定了9种酱油,并与文献报道的高效液相色谱法的结果进行比较,结果满意。     

毛细管电泳法分离检测饮料中的防腐剂

采用高效毛细管电泳法,同时在线分离检测对羟基苯甲酸甲酯、山梨酸钾和苯甲酸3种防腐剂。考察了运行缓冲液的浓度、pH值、分离电压、进样时间等因素对电泳分离的影响。在检测波长为230nm时,获得了3种防腐剂分离检测的最优化实验条件为:20mmol/L pH 9.2的硼砂缓冲溶液,分离电压为22kV,进样时间15s。在最优化实验条件下,3种防腐剂检测的线性相关系数均大于0.98,检出限为1.0×10-2g/kg。利用此方法检测了市售3种饮料中所含防腐剂的种类和含量,各种防腐剂的回收率在88%~102%之间。