Flow injection potentiometric determination of saccharin in dietary products with relocation of filtration unit

A flow injection potentiometric procedure for saccharin determination in dietary products is proposed. Saccharin is precipitated as mercurous saccharinate and the excess of the mercurous cation is potentiometrically measured using a silver wire coated with a mercury film as the working electrode. A filter unit is used to avoid contact between the precipitate and the electrode surface. With relocation in the flow manifold, the accumulated precipitate is removed on-line. Sucrose, glucose, aspartame, sodium cyclamate and sodium benzoate do not interfere when present in amounts similar to those observed in commercial products. Results are comparable with those obtained by UV-spectrophotometry and the correlation coefficient between methods is equal to 0.9930. A linear relationship between DeltaE (mV) and the logarithm of saccharin concentration was obtained in the saccharin concentration range 2 x 10(-3) - 1 x 10(-2)M. The sampling frequency is 60/hour and only 0.76 mg of Hg(2+)(2) is consumed in each determination.     

A simple turbidimetric flow injection system for saccharin determination in sweetener products

A new method for saccharin determination in liquid sweetener products was developed. The method is based on the precipitation reaction of Ag(I) ions with saccharin in aqueous medium (pH 3.0), using a flow injection analysis system with merging zones, the suspension was stabilized with 5 g L⁻¹ Triton X-100. All experimental parameters influencing the flow injection system were optimized by means of chemometric approaches. The linear analytical curve was built from 2.4 g L⁻¹ up to 9.64 g L⁻¹ (r = 0.9968) with a quantification limit of 2.40 g L⁻¹. The precision assessed as relative standard deviation (n = 10) was found to be 1.75 % for the saccharin concentration of 7.20 g L⁻¹. Based on interference studies performed with the substances commonly found in liquid sweeteners, such as sodium cyclamate, methylparaben, sodium aspartame, and benzoic and citric acids, at the analyte to interferent mole ratio of up to 1: 10, no interference with the saccharin determination was observed. The presence of chloride ions interferes with the method, but a preceding liquid-liquid saccharin extraction with ethyl acetate was successfully employed to overcome this drawback. Accuracy of the method in sweetener products was evaluated by a comparison with the HPLC method.     

乳及乳制品中多种防腐剂和甜味剂的同时测定

建立了高效液相色谱法同时测定乳及乳制品中安赛蜜、苯甲酸、糖精钠、山梨酸和阿斯巴甜的方法。通过加入适量沉淀剂除去样品中绝大部分蛋白质后,采用C18色谱柱分离,以甲醇-0.05 mol/L磷酸二氢钾溶液为流动相梯度洗脱,用二极管阵列检测器于230 nm波长处检测安赛蜜、苯甲酸和山梨酸,于210 nm波长处检测糖精钠和阿斯巴甜。被测物的回收率为96.0%～103.5%,精密度(以相对标准偏差(RSD)计)为1.93%～2.76%,安赛蜜、苯甲酸、糖精钠、山梨酸和阿斯巴甜的检出限分别为1.0, 1.0, 0.5, 1.0, 1.5 μg/g。该方法可用于乳及乳制品中这5种添加剂的同时测定。     

高效液相色谱法测定镍镀液中的糖精钠和苯亚磺酸钠

建立了高效液相色谱法同时测定镍镀液中常用光亮剂苯亚磺酸钠和糖精钠的定量检测方法.为避免高盐背景对色谱分析的干扰,研究了样品的除盐处理方法.对方法的线性关系、回收率、精密度进行验证,并利用方法测定电镀液中苯亚磺酸钠和糖精钠,得到其实际消耗曲线:在400 A/m2的电流密度条件下苯亚磺酸钠4 h内平均消耗速率为18.25 ...     

表面增强拉曼光谱法快速测定干果类食品中的糖精钠

建立了干果中糖精钠的表面增强拉曼光谱(SERS)快速分析方法。干果样品经水提取、C18固相萃取柱净化除杂后进行表面增强拉曼光谱分析。该方法的线性范围为50.0~250 mg/L,检出限为0.6 g/kg,回收率为80.0%~125%,相对标准偏差(RSD,n=5)不大于8.4%。结果表明该方法灵敏度高、杂质干扰小、准确度高,满足干果类食品中糖精钠的快速检测要求,在干果类食品安全质量监控方面具有良好的应用潜力。     

Sweeteners determination in table top formulations using FT-Raman spectrometry and chemometric analysis

A partial least squares (PLS) Fourier transform Raman spectrometry procedure based on the measurement of solid samples contained inside standard glass vials, has been developed for direct and reagent-free determination of sodium saccharin and sodium cyclamate in table top sweeteners. A classical 2² design for standards was used for calibration, but this system provides accuracy errors higher than 13% w/w for the analysis of samples containing glucose monohydrate. So, an extended model incorporating glucose monohydrate (2³ standards) was assayed for the determination of sodium saccharin and sodium cyclamate in all the samples. Mean centering spectra data pre-treatment has been employed to eliminate common spectral information and root mean square error of calibration (RMSEC) of 0.0064 and 0.0596 was obtained for sodium saccharin and sodium cyclamate, respectively. A mean accuracy error of the order of 1.1 and 1.9% w/w was achieved for sodium saccharin and sodium cyclamate, in the validation of the method using actual table top samples, being lower than those obtained using an external monoparametric calibration. FT-Raman provides a fast alternative to the chromatographic method for the determination of the sweeteners with a three times higher sampling throughput than that obtained in HPLC. On the other hand, FT-Raman offers an environmentally friendly methodology which eliminates the use of solvents. Furthermore, the stability of samples and standards into chromatographic standard glass vials allows their storage for future analysis thus avoiding completely the waste generation.     

糖精钠与牛血清白蛋白相互作用的荧光光谱研究

在模拟人体生理条件下,应用荧光和紫外-可见光谱法研究了糖精钠与牛血清白蛋白(BSA)之间的相互作用;并计算了不同温度下的热力学参数、结合常数和结合位点数.结果表明,糖精钠对BSA的猝灭机制属于形成复合物的静态猝灭过程;两者之间的作用主要是氢键或范德华力,作用的位点更靠近色氨酸;金属离子对两者的作用具有一定的影响.     

高效离子排斥色谱法测定饮料中的糖精钠

提出了一种用高效离子排斥色谱法测定饮料中糖精钠的新方法。以ＩｏｎＰａｃ ＩＣＥ－ＡＳ ６柱为分离柱，０．１０ ｍｍｏｌ／ＬＨ２ＳＯ４＋甲醇（９＋１）为淋洗液，２０２ｎｍ波长下紫外检测。在１－１００ｍｇ／Ｌ范围内，糖精钠的含量与峰面积呈 良好线性关系。检出限为０．６０ｎｇ，灵敏度优于以往采用离子交换色谱－电导检测法的结果。在实验条件下，饮料 中常见有机酸以及其它人工合成甜味剂等均不产生干扰。方法用于饮料中糖精钠的测定，加标回收率为９８％～ １０５％。此外还比较了电导检测、紫外检测和经化学抑制系统后紫外检测等三种检测方式对测定灵敏度的影响。     

固相萃取-高效液相色谱-可变波长检测法同时测定调味品中甜味剂和人工合成色素

建立了同时测定调味品中糖精钠和合成色素的固相萃取-高效液相色谱(SPE-HPLC)分析方法。样品经石油醚低温去除油脂,聚酰胺固相萃取柱净化和富集,然后进行HPLC分析。采用反相C₁₈色谱柱,以甲醇和0.02 mol/L醋酸铵为流动相进行梯度洗脱,使用可变波长分别在230、510、484和510 nm进行检测。实验结果表明:糖精钠与合成色素的分离效果良好,回收率为88.6%～97.1%,相对标准偏差小于5%;方法检出限均可达到0.05 mg/kg。该方法操作简单,结果准确可靠,重现性好,适用于大批量调味品中甜味剂和人工合成色素的同时检测。     

Simultaneous determination of sweeteners and preservatives in preserved fruits by micellar electrokinetic capillary chromatography

A micellar electrokinetic capillary method for the simultaneous determination of the sweeteners dulcin, aspartame, saccharin, and acesulfame-K and the preservatives sorbic acid; benzoic acid; sodium dehydroacetate; and methyl-, ethyl-, propyl-, isopropyl-, butyl-, and isobutyl-p-hydroxybenzoate in preserved fruits is developed. These additives are ion-paired and extracted using sonication followed by solid-phase extraction from the sample. Separation is achieved using a 57-cm fused-silica capillary with a buffer comprised of 0.05 M sodium deoxycholate, 0.02 M borate-phosphate buffer (pH 8.6), and 5% acetonitrile, and the wavelength for detection is 214 nm. The average recovery rate for all sweeteners and preservatives is approximately 90% with good reproducibility, and the detection limits range from 10 to 25 microg/g. Fifty preserved fruit samples are analyzed for the content of sweeteners and preservatives. The sweeteners found in 28 samples was aspartame (0.17-11.59 g/kg) or saccharin (0.09-5.64 g/kg). Benzoic acid (0.02-1.72 g/kg) and sorbic acid (0.27-1.15 g/kg) were found as preservatives in 29 samples.     

HPLC-Bestimmung polarer Verunreinigungen in Saccharin und Saccharin-Natrium

Zusammenfassung Eine HPLC-Methode wird beschrieben zur direkten Bestimmung polarer Verunreinigungen in Saccharin und Saccharin-Natrium, o- und p-Sulfobenzoesäure sowie o- und p-Sulfamoylbenzoesäure lassen sich bis zu einer Nachweisgrenze von 1 mg/kg bestimmen. Für eine Konzentration von 10 mg/kg beträgt die Standardabweichung 0,4 mg/kg.Eine tabellarische Zusammenfassung der Ergebnisse von handelsüblichen Saccharin-Qualitäten wird unter Hinweis auf das Herstellungsverfahren gegeben.

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Determination of polar impurities in saccharin and saccharin sodium by HPLC

Summary A HPLC method for the direct determination of polar impurities in saccharin and saccharin sodium is described, o- and p-Sulphobenzoic acid as well as o- and p-sulphamoylbenzoic acid can be detected down to a limit of 1 mg/kg. For a concentration of 10 mg/kg the standard deviation is 0.4 mg/kg.A tabulated summary of the results obtained from commercial saccharin qualities is given with reference to the manufacturing process.

     

Determination of Artificial Sweeteners by High-Performance Ion-Mobility Spectrometry with Electrospray Ionization

There are increasing demands for simple, rapid, low-cost, and green methods for the determination of artificial sweeteners that are of concern because of their toxicity. Acesulfame-K, sodium saccharin, sodium cyclamate, aspartame, and neotame were determined by high-performance ion-mobility spectrometry with direct electrospray ionization (ESI-HPIMS). The resolving power exceeded 60 in both positive- and negative-ion modes. The single acquisition time was less than 10?s and the total analysis time was under 2?min which is faster than traditional chromatography methods. Calibration curves were established for the sweeteners at concentrations from 0.1 to 1.5 or 2.0?mg/L with correlation coefficients of approximately 0.99. The combination of simple sample preparation, fast analysis, high sensitivity, robustness, green properties, and low cost makes ESI-HPIMS a promising technique for the determination of acesulfame-K, sodium saccharin, sodium cyclamate, aspartame, and neotame in water and beverages.     

固相萃取-高效液相色谱-蒸发光散射检测法同时检测食品中5种人工合成甜味剂

建立了高效液相色谱-蒸发光散射检测仪(HPLC-ELSD)同时检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖和阿斯巴甜5种甜味剂的方法。甜味剂经0.1%(v/v)甲酸缓冲液提取后,利用C18固相萃取小柱净化浓缩,以3 μm C18柱为分离柱,0.1%(v/v)甲酸(氨水调节pH=3.5)-甲醇(61:39, v/v)为流动相,经高效液相色谱法分离,蒸发光散射检测器进行检测。结果表明,5种甜味剂在30～1000 mg/L的范围内,具有良好的线性关系(相关系数大于0.997);在3个添加水平下,样品的平均回收率为85.6%～109.0%,相对标准偏差小于4.0%;方法检出限(LOD,信噪比(S/N)=3)分别为安赛蜜2.5 mg/L、糖精钠3 mg/L、甜蜜素10 mg/L、三氯蔗糖2.5 mg/L及阿斯巴甜5 mg/L。该方法简单、灵敏、操作成本低,可用于不同形态食品中多种甜味剂的同时检测。     

Studies on Synthesis of Novel Triazole Tagged Pyrazole Fused Naphthalene 5‐Thiazine‐5,5‐dioxide Derivatives,Their Antimicrobial,and Antioxidant Activity

A series of novel triazole tagged pyrazole fused naphthalene‐5‐thiazine‐5,5‐dioxide derivatives 8 and 9 were synthesized starting from sodium salt of saccharin 1 . The structure of each intermediate and products was established on the basis of spectroscopy data. All the synthesized compounds 8 and 9 were screened against various bacterial and fungal strains but found to show no activity up to 150‐µg/mL concentration. Further screening for antioxidant property resulted promising compounds.     

HPLC analysis of aspartame and saccharin in pharmaceutical and dietary formulations

Summary A reversed-phase HPLC method has been developed suitable for a reliable quality control of pharmaceutical and dietary formulations containing the synthetic sweeteners aspartame and saccharin. The proposed method is able to separate acesulfame, aspartame and saccharin, and their impurities such as 5-benzyl-3,6-dioxo-2-piperazineacetic acid (the major degradation product of aspartame) and 4-sulphamoylbenzoic acid,o- andp-toluenesulphonamides (the synthesis impurities of saccharin). A convenient solid-phase extraction (SPE) procedure using C-18 sorbent, was also developed for the determination of potential saccharin impurities.     

Facile synthesis of 1, 2‐benzisothiazole‐3‐one‐1,1 ‐dioxide methylsulfonyl derivatives

An improved and general synthesis of saccharin methylthio and methylsulfone derivatives from chlorosubstituted saccharins is presented. A large‐scale procedure for preparation of chloro‐substituted saccharins was developed. Treatment of the saccharin chlorides with sodium thiomethoxide and t‐BuOK in DMF gave the saccharin methyl sulfides, which upon chromium(VI) oxide catalyzed oxidation with periodic acid afforded the corresponding saccharin methylsulfones in high yields.     

Detection of counterfeit stevia products using a handheld Raman spectrometer

Stevia is a highly appreciated natural sweetener because it can be consumed by diabetic patients. Due to the increasing popularity of stevia during the last years, counterfeit products have been making their way into the market. Raman spectroscopy is a versatile analytical technique that can be used for control tasks and handheld modern devices expand its possible applications to instant in situ measurements. The Raman spectra of six commercial stevia products (five purchased in Bolivia and one in Germany) were recorded and compared to the spectra of standards of rebaudioside A and stevioside as well as the spectra of the artificial sweeteners sodium cyclamate and sodium saccharin. Based on the Raman spectroscopic data, it was verified that three of the Bolivian products were counterfeit products and another one was rich in maltodextrin. The Raman spectra of one Bolivian product and the German one revealed rebaudioside A and stevioside as major components. Raman spectroscopy was capable of detecting contents as low as 5% (w/w) of sodium cyclamate during measurements of stevia-sodium cyclamate mixtures. The results show that Raman spectroscopy can successfully be used to detect counterfeit stevia and underline its high potential for the detection of food adulteration.     

荧光分子探针在糖精钠检测中的应用

随着科技的发展和社会的进步,食品安全问题越来越受到关注。糖精钠作为一种食品添加剂,其非法添加事件时有发生,因此,有必要找到一种快速准确检测糖精钠的方法。荧光分子探针因具有灵敏度高、选择性好、响应时间短的优点,其在分析化学检测中的应用越来越广泛。本文设计并合成了一种含蒽荧光团的氮杂15-冠-5化合物,利用分子识别的原理,该目标化合物能够特异性识别溶液中的糖精钠,使溶液的荧光强度发生变化,具有肉眼可见、易于观察的特点,该方法为食品中糖精钠的快速检测提供了一种可行的手段。     

Spectrophotometric determination of saccharin in different materials by a solvent extraction method using Nile Blue as reagent

In a slightly acidic medium (sodium acetate-acetic acid buffer, pH 4) saccharin and Nile Blue form an ion-association compound which is extractable into methyl isobutyl ketone and allows the spectrophotometric determination of saccharin. At 630 nm Beer's law is obeyed over the saccharin concentration range 0.1-3.5 microg/ml in the aqueous phase and the apparent molar absorptivity is 5.8 x 10(4) l.mole(-1).cm(-1). The method shows good selectivity and can be applied to the determination of saccharin in artificial sweeteners, soft drinks and toothpastes.     

高效液相色谱-串联质谱法测定食品中6种人工合成甜味剂

建立了食品中6种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜、阿斯巴甜、阿力甜、纽甜)的高效液相色谱-串联质谱检测方法。样品经甲醇-水溶液(1:1, v/v)提取,以C18柱为分离柱,0.1%(v/v)甲酸-5 mmol/L甲酸铵溶液/乙腈为流动相,经高效液相色谱分离,采用电喷雾串联四极杆质谱进行检测。结果表明,6种人工合成甜味剂在20～500 μg/L范围内定量离子对的响应峰面积和样品质量浓度之间有良好的线性关系(相关系数＞0.998)。在3个添加水平下,样品平均回收率为81.3%～106.0%,相对标准偏差小于11%。该方法简单、灵敏、准确,可用于食品中6种人工合成甜味剂的同时检测。