Formulation optimisation of a whey lemon beverage using a blend of the sweeteners aspartame and saccharin

Product formulations based on combinations of two sweeteners were optimised in a sweetened paneer whey lemon beverage (WLB) by organoleptic panels. The binary sweetener blend aspartame/saccharin (70:30, 0.0425%) scored the highest based upon comparison with the best‐optimised single sweetener aspartame (0.07%) in WLB and had nonsignificant differences with the control WLB sweetened with sucrose in all sensory attributes. This best binary blend showed maximum synergy in sweetness intensity (14.4%) and overall acceptability (7.5%) in respect of a single sweetener aspartame. The multiple‐sweetener approach involving use of binary blend (0.0425%) resulted in 39% reduction of usage level when compared with single sweetener aspartame (0.07%).     

反相高效液相色谱法同时测定饮料中安赛蜜 苯甲酸 山梨酸 糖精钠

采用反相HPLC法，探讨了在同一色谱条件下，饮料中安赛蜜、苯甲酸、山梨酸及糖精钠的分离测定条件。采用ZORBAX Eclipse XDB—C18柱，以0．02mol／L甲醇-乙酸铵（体积比为8：92）为流动相，流速为1．0mL／min，检测波长230nm。该法简便、快速、重现性好、回收率高。     

Simultaneous determination of aspartame,cyclamate, saccharin and acesulfame-K in soft drinks and tabletop sweetener formulations by capillary electrophoresis with capacitively coupled contactless conductivity detection

Capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C⁴D) was used for simple, rapid, and simultaneous determination of aspartame, cyclamate, saccharin and acesulfame-K in commercial samples of soft drinks and tabletop sweetener formulations. A buffer solution containing 100 mmol L⁻¹ tris(hydroxymethyl)aminomethane (TRIS) and 10 mmol L⁻¹ histidine (His) was used as background electrolyte (BGE). A complete separation of the analytes could be attained in less than 6 min. The limits of detection (LOD) and quantification (LOQ) were considered better than those usually obtained by CE with photometric detection. Recoveries ranging from 94% to 108% were obtained for samples spiked with standard solutions of the sweeteners. The relative standard deviation (RSD) for the analysis of the samples with the CE-C⁴D method varied in the range of 1.5%–6.5%.     

UPLC/MS/MS法测定饮料中甜蜜素、糖精钠和安赛蜜

建立了超高效液相色谱-串联质谱法(ultra high-performance liquid chromatography-tandem massspectrometry,UHPLC-MS/MS)测定饮料中甜蜜素、糖精钠和安赛蜜的检测方法。饮料加水稀释涡旋,用N-丙基乙二胺(PSA)净化样品,经0.22μm微孔滤膜过滤后测定甜蜜素;用乙酸锌-亚铁氰化钾净化样品,经0.22μm微孔滤膜过滤后测定糖精钠和安赛蜜。甜蜜素和安赛蜜在5～200μg/L、糖精在20～200μg/L范围内线性关系良好,方法检出限(S/N=3)为0.2～10μg/kg,方法定量限(S/N=10)为0.6～30μg/kg,3种化合物在奶茶中加标回收率为78.9%～95.7%,果茶中加标回收率为80%～102%。方法操作简单,检出限低,重现性好,回收率良好,干扰小。     

高效液相色谱法同时测定可乐中苯甲酸、糖精钠、安赛蜜和咖啡因

目的建立高效液相色谱同时测定可乐中苯甲酸、糖精钠、安赛蜜和咖啡因的方法,并应用于国际FAPAS能力验证。方法样品经超声脱气用水稀释,采用C_(18)色谱柱分离,以乙酸铵缓冲液(0.02 mol/L)/甲醇为流动相,采用梯度洗脱分离,在230 nm、272 nm波长下进行检测。结果苯甲酸、糖精钠、安赛蜜和咖啡因线性范围为2.0~200μg/m L,线性关系良好,相关系数大于0.999,回收率在97%~103%之间,RSD为0.5%~2.8%之间,检出限在0.005~0.02μg/m L之间。结论该法灵敏度高、重现性好,用于FAPAS能力验证时结果接近中值。     

Estimated intake of the artificial sweeteners acesulfame-K, aspartame, cyclamate and saccharin in a group of Swedish diabetics.

Few sweetener intake studies have been performed on the general population and only one study has been specifically designed to investigate diabetics and children. This report describes a Swedish study on the estimated intake of the artificial sweeteners acesulfame-K, aspartame, cyclamate and saccharin by children (0-15 years) and adult male and female diabetics (types I and II) of various ages (16-90 years). Altogether, 1120 participants were asked to complete a questionnaire about their sweetener intake. The response rate (71%, range 59-78%) was comparable across age and gender groups. The most consumed 'light' foodstuffs were diet soda, cider, fruit syrup, table powder, table tablets, table drops, ice cream, chewing gum, throat lozenges, sweets, yoghurt and vitamin C. The major sources of sweetener intake were beverages and table powder. About 70% of the participants, equally distributed across all age groups, read the manufacturer's specifications of the food products' content. The estimated intakes showed that neither men nor women exceeded the ADI for acesulfame-K; however, using worst-case calculations, high intakes were found in young children (169% of ADI). In general, the aspartame intake was low. Children had the highest estimated (worst case) intake of cyclamate (317% of ADI). Children's estimated intake of saccharin only slightly exceeded the ADI at the 5% level for fruit syrup. Children had an unexpected high intake of tabletop sweeteners, which, in Sweden, is normally based on cyclamate. The study was performed during two winter months when it can be assumed that the intake of sweeteners was lower as compared with during warm, summer months. Thus, the present study probably underestimates the average intake on a yearly basis. However, our worst-case calculations based on maximum permitted levels were performed on each individual sweetener, although exposure is probably relatively evenly distributed among all sweeteners, except for cyclamate containing table sweeteners.     

Usage of saccharin in food products and its intake by the population of Lucknow, India

A survey of the usage patterns of the artificial sweetener, saccharin, in edible products and a study of its intake pattern in different population groups has been carried out. Of the different edible commodities, ice candy (87 samples) and crushed ice (14 samples), commonly consumed by children, and pan masala (16 samples) and pan flavourings (10 samples), consumed by the habitual population, were collected from different areas of Lucknow, India. Saccharin was extracted from the samples according to an AOAC method and analysed by HPLC. The consumption pattern of ice candy and crushed ice was determined for 6-20 year olds from a household dietary survey using the food frequency recall method (414 families having 1039 subjects). The consumption of pan masala and pan was assessed by a survey of habitual adult consumers comprising 782 and 1141 subjects, respectively. The average and maximum amounts of saccharin in pan masala samples were 12 750 and 24 300 mg kg^-1, respectively, which are 1.6- and 3-fold higher than the maximum permitted levels allowed under Prevention of Food Adulteration (PFA) Act of India. In pan flavourings, the average and maximum amount of saccharin was 12.2 and 20.1%, i.e. 1.52- and 2.5-fold higher than the permissible limits of the PFA Act. The samples of ice candy and crushed ice showed average and maximum levels of 200 and 700 mg kg^-1 and 280 and 460 mg kg^-1, respectively. The average intake of saccharin through ice candy and crushed ice was less than 21% of the acceptable daily intake (ADI) (5 mg kg^-1 body weight (bw) day^-1). However, the maximum intake of saccharin, especially in the 6-10-year age group, contributed 57 and 68% of the ADI through ice candy and crushed ice, respectively. Maximum consumption of saccharin in all the age groups, if consuming both ice candy and crushed ice, results in exceeding the ADI by 54% for subjects in the 6-10-year age group. Hence, the 6-10-year age group population may be at risk of exceeding the ADI for saccharin. The average and maximum theoretical daily intake of saccharin through pan masala alone was 1.84 and 13.33 mg kg^-1 bw day^-1, contributing 37 and 267% of the ADI, whereas the estimated (maximum) daily intake was 810% of the ADI. The estimated maximum daily intake (EDI) of saccharin through pan was 6.87 mg kg^-1 bw day^-1, which was 137% of the ADI. Thus, individuals in the maximum consumption group for pan masala or pan may be susceptible to toxic effects of saccharin, including bladder distention, elevated urine osmolality and bladder cancer.     

Metabolic effects of aspartame in adulthood: A systematic review and meta-analysis of randomized clinical trials

Data about harms or benefits associated with the consumption of aspartame, a nonnutritive sweetener worldwide consumed, are still controversial. This systematic review and meta-analysis of randomized controlled clinical trials aimed to assess the effect of aspartame consumption on metabolic parameters related to diabetes and obesity. The search was performed on Cochrane, LILACS, PubMed, SCOPUS, Web of Science databases, and on a gray literature using Open Grey, Google Scholar, and ProQuest Dissertations &; Theses Global. Searches across all databases were conducted from the earliest available date up to April 13, 2016, without date and language restrictions. Pooled mean differences were calculated using a random or fixed-effects model for heterogeneous and homogenous studies, respectively. Twenty-nine articles were included in qualitative synthesis and twelve, presenting numeric results, were used in meta-analysis. Fasting blood glucose (mmol/L), insulin levels (μU/mL), total cholesterol (mmol/L), triglycerides concentrations (mmol/L), high-density lipoprotein cholesterol (mmol/L), body weight (kg), and energy intake (MJ) were considered as the main outcomes in subjects that consumed aspartame, and results were presented as mean difference; % confidence interval, range. Aspartame consumption was not associated with alterations on blood glucose levels compared to control (?0.03 mmol/L; 95% CI, ?0.21 to 0.14) or to sucrose (0.31 mmol/L; 95% CI, ?0.05 to 0.67) and on insulin levels compared to control (0.13 μU/mL; 95% CI, ?0.69 to 0.95) or to sucrose (2.54 μU/mL; 95% CI, ?6.29 to 11.37). Total cholesterol was not affected by aspartame consumption compared to control (?0.02 mmol/L; 95% CI, ?0.31 to 0.27) or to sucrose (?0.24 mmol/L; 95% CI, ?0.89 to 0.42). Triglycerides concentrations were not affected by aspartame consumption compared to control (0.00 mmol/L; 95% CI, ?0.04 to 0.05) or to sucrose (0.00 mmol/L; 95% CI, ?0.09 to 0.09). High-density lipoprotein cholesterol serum levels were higher on aspartame compared to control (?0.03 mmol/L; 95% CI, ?0.06 to ?0.01) and lower on aspartame compared to sucrose (0.05 mmol/L; 95% CI, 0.02 to 0.09). Body weight did not change after aspartame consumption compared to control (5.00 kg; 95% CI, ?1.56 to 11.56) or to sucrose (3.78 kg; 95% CI, ?2.18 to 9.74). Energy intake was not altered by aspartame consumption compared to control (?0.49 MJ; 95% CI, ?1.21 to 0.22) or to sucrose (?0.17 MJ; 95% CI, ?2.03 to 1.69). Data concerning effects of aspartame on main metabolic variables associated to diabetes and obesity do not support a beneficial related to its consumption.     

高效液相色谱法同时测定食品中安赛蜜、苯甲酸、山梨酸、糖精钠以及脱氢乙酸

建立食品中安赛蜜、苯甲酸、山梨酸、糖精钠、脱氢乙酸等甜味剂和防腐剂的高效液相色谱测定法。方法采用C18(5um,4.6mm×150mmi.d)反相色谱柱,流动相:v(甲醇)∶v(0.02moL/L乙酸铵溶液)=(5∶95),流速1.0mL/min,检测波长230nm,柱温30℃,进样量5μL。样品的检出限1.5～4.4mg/kg,线性范围1～10mg/L,加标回收率95.5%～103.6%,相对标准偏差为0.95%～2.81%(n=6)。该法具有样品预处理简单,灵敏度高,分析时间短等优点,可用于食品样品的直接测定。     

Daily intake assessment of saccharin, stevioside, D-sorbitol and aspartame from various processed foods in Korea

This study was carried out to estimate the daily intakes (EDIs) of artificial sweeteners such as saccharin, stevioside, D-sorbitol and aspartame in order to evaluate the safety of the artificial sweeteners in Korea. A total of 274 food samples were selected from the foods considered to be representative sources of artificial sweeteners in the Korean diet and analysed by using HPLC with evaporative light scattering and ultraviolet detectors. In case of aspartame, the reference values were used without instrumental analysis. The EDIs of saccharin, stevioside, D-sorbitol and aspartame for average consumers were 0.028, 0.008, 4.9 and 0.14 mg kg^-1 body weight day^-1, respectively, and as a proportion of the acceptable daily intake (ADI) were not higher than 1% of ADI of the Joint FAO/WHO Expert Committee on Food Additives (JECFA). For 90th percentile consumers, the EDIs of saccharin, stevioside, D-sorbitol and aspartame were 2.0, 0.20, 141 and 4.6 mg kg^-1 body weight day^-1, respectively, and as a proportion of the ADI, the EDIs of saccharin and aspartame were 40.7% and 11.4% of the ADI set by the JECFA, respectively. Because JECFA did not assign ADIs for stevioside and D-sorbitol, the values for these sweeteners were not compared. According to these results, the EDIs of artificial sweeteners such as saccharin and aspartame in Korea are significantly lower than ADI set by the JECFA.     

RP-HPLC法同时测定糕点中安赛蜜、苯甲酸、山梨酸、糖精钠和脱氢乙酸

建立反相高效液相色谱法(RP-HPLC同时测定糕点中安赛蜜、苯甲酸、山梨酸、糖精钠和脱氢乙酸。该方法糕点样品经处理后,采用SunFire C185μ4.6 mmmm反相色谱柱,流动相为甲醇:磷酸盐缓冲液(pH6.7=793等度洗脱,流速为1.0 mL/min检测波长230 nm柱温为30℃进样量为20μ。线性范围0.2 mg/L120 mg/L检出限0.4 mg/kg1.0 mg/kg加标回收率为87.7%105.3%相对标准偏差小于5%。结果表明,该方法操作简便、结果可靠,可用于同时检测糕点中安赛蜜、苯甲酸、山梨酸、糖精钠和脱氢乙酸。     

富硒豆豉中安赛蜜、苯甲酸、山梨酸、糖精钠、 脱氢乙酸的测定

目的建立高效液相色谱法同时测定富硒豆豉中安赛蜜、苯甲酸、山梨酸、糖精钠和脱氢乙酸的分析方法。方法样品经过沉淀剂沉淀蛋白后过滤,使用C_(18)反向色谱柱(pH1.5～9.0)分离,用甲醇-乙酸铵溶液作为流动相进行洗脱,经高效液相色谱紫外检测器和二极管阵列检测器检测,检测波长为230 nm。结果 5种添加剂具有良好的线性关系,相关系数均大于0.9990,检出限为1.0～2.0mg/kg。应用该方法检测富硒豆豉的加标回收率为90.2%～101.1%,相对标准偏差小于2.0%。结论本研究建立的方法有效可行,结果可靠,适用于富硒豆豉中5种添加剂的检测。     

高效液相色谱法同时检测酸性乳饮料及冰淇淋中安赛蜜、苯甲酸、山梨酸和糖精钠含量

目的建立酸性乳饮料及冰淇淋中安赛蜜、苯甲酸、山梨酸、糖精钠含量的高效液相色谱分析方法。方法样品去除蛋白后,用甲醇提取,提取液用高压液相色谱仪进行检测。结果安赛蜜、苯甲酸、山梨酸、糖精钠在0~100μg/kg范围内,浓度与峰面积有良好的线性关系,相关系数大于0.999,检出限分别为2.87、0.96、0.97和2.69 mg/kg;样品的加标平均回收率分别为95.59%~104.52%、93.21%~108.05%、97.75%~107.98%和97.48%~103.67%,相对标准偏差均小于10%。结论本方法适用于酸性乳饮料及冰淇淋中安赛蜜、苯甲酸、山梨酸、糖精钠含量同时测定的需要。     

高效液相色谱法同时检测黄油及无水奶油中苯甲酸、山梨酸、安赛蜜、糖精钠

目的建立黄油及无水奶油中2种甜味剂(安赛蜜、糖精钠)及2种防腐剂(苯甲酸、山梨酸)含量的高效液相色谱分析方法。方法样品去除脂肪后,用甲醇-水(1:1,V:V)提取,提取液使用C8色谱柱(250mm×4.6 mm, 5μm)、在波长为230 nm、流动相为1.0 mL/min的条件下进行检测。结果苯甲酸、山梨酸、安赛蜜、糖精钠在0～100μg/mL范围内,浓度与峰面积有良好的线性关系,相关系数大于0.99,检出限分别为0.87、0.91、2.75、2.91 mg/kg;样品的加标平均回收率分别为93.12%～102.34%、93.02%～103.23%、91.53%～108.16%、93.48%～105.46%,相对标准偏差均小于10%。结论本方法可适用于黄油及无水奶油中苯甲酸、山梨酸、安赛蜜、糖精钠含量同时测定。     

Occurrence of caffeine,saccharin, benzoic acid and sorbic acid in soft drinks and nectars in Portugal and subsequent exposure assessment

A reliable method for the determination of benzoic and sorbic acids, caffeine and saccharin in soft drink and nectars using high performance liquid chromatography and UV detection was validated. The chromatographic separation was achieved with a C18 column (250 × 4.6 mm) and one buffered mobile phase, KH₂PO₄ 0.02 M/ACN (90:10)/phosphoric acid at pH 4.2. The effluent was monitored at 220 nm.     

Simultaneous determination of sodium saccharin,aspartame, acesulfame-K and sucralose in food consumed in Korea using high-performance liquid chromatography and evaporative light-scattering detection

ABSTRACT

Four artificial sweeteners, i.e., sodium saccharin, aspartame, acesulfame-K and sucralose, are permitted for use in Korea, and recent regulatory changes have expanded the number of food categories in which they may be used. Four artificial sweeteners were determined simultaneously in more than 900 food items from 30 food categories that are commercially available in Korean markets, including both domestic and imported products, using high-performance liquid chromatography and evaporative light-scattering detection (ELSD). A new procedure using 75% acetone to remove fat was applied for sample preparation. The levels detected in all samples were below the maximum permitted use levels established in Korea. Despite the increased number of categories, the only one in which sodium saccharin was newly found was takju, an alcoholic beverage. Sodium saccharin was not found in other beverages in the food analysis or in the food label survey, even though its use was reported in a previous study, suggesting that consumer preference outweighs regulatory decisions. When the analytical results were combined with food-consumption data obtained from the Korea National Health and Nutrition Examination Survey 2010–14, the estimated daily intakes of all the sweeteners were considered safe.     

高压液相色谱法同时测定食品中的维生素A、D、E和K

本方法研究了应用反相高压液相色谱技术,同时测定食品中的维生素A、D、E、K。以C18柱为固定相(μ Bondapak C18,30cm×4mm),甲醇作流动相。在290nm下测定维生素A、E,在265nm下测定维生素D、K。样品的前处理分为两种,第一种皂化法,可同时测定维生素A、D、E。加标样品的回收率分别为:V_A97.2～110％,V_D92.3～102％,V_E96.6～110％。变异系数(CV％)分别为V_A2.29～3.15％,VD5.99～8.63％,V_E3.60～4.16％。第二种为酶解法,可同时测定维生素A、D、E、K四种,加标样品的回收率分别为:V_A87.62～98.01％,V_D90.23～102.7％,V_E86.18～91.09％,V_K80.15～85.07％。变异系数(CV％)分别为:V_A5.51％,V_D8.87％,V_E4.91％,V_K3.67％。     

FT-NIR光谱法同时测定烟草根、茎、叶中的氮、磷、氯和钾

应用傅里叶变换近红外(FT NIR)光谱法测定了1210个具代表性的烤烟各个生长期的根、茎、叶样品的近红外光谱数据,并采用偏最小二乘法(PLS)分别对实验数据进行处理,建立了预测根茎和烟叶氮、磷、氯和钾等主要营养元素含量的校正模型。通过对模型进行数理统计检验,在显著性水平大于5%的条件下,其预测值与测定值不存在显著性差异。     

火焰原子光谱法测定湘玉竹中的钾钙铜

玉竹作为一种药、食两用草本植物,具有独特的营养与保健功能,近几年来受到了人们的广泛关注。探讨产自湖南的玉竹样品的前处理与试液制备,利用火焰原子光谱法测定湘玉竹中的金属元素钾、钙、铜。考察硝酸、过氧化氢和高氯酸的影响,以及在同一体系中钾、钙、铜的干扰情况。在选定的条件下,钾、钙、铜的检出限分别为0.03μg/g、0.04μg/g、0.03μg/g。钾、钙、铜的相关系数分别为0.9992、0.9998、0.9978,回收率分别为96.6%￣99.2%、97.3￣98.9%、96.8%￣97.5%。相对标准偏差分别为0.9%￣3.1%。结果表明,火焰原子光谱法测定湘玉竹中的钾、钙、铜,快速、简便、经济,而且干扰少,测得的结果令人满意。     

Corn bran versus corn grain at 2 levels of forage: Intake,apparent digestibility,and production responses by lactating dairy cows

The objective of this study was to determine the effect of substituting corn bran (CB) for dried ground corn grain (CG) in the nonforage portion of high-forage (HF) and low-forage (LF) diets. Twelve multiparous and 12 primiparous Holsteins were assigned to 4 diets using six 4 ×  Latin squares with 3-wk periods. Forage was 64 or 38% of the total mixed ration (% of dry matter). On a dry matter basis, the HFCG diet had 20% CG, the LFCG diet had 39% CG, the HFCB diet had 19% CB, and the LFCB diet had 38% CB. Digestible organic matter intake (OMI) and milk energy yield were lower for CB compared with CG within forage level. Digestible OMI was greater (1.9 kg/d) for the LFCG compared with the HFCG treatment. When CB replaced forage (LFCB vs. HFCB), digestible OMI was not different but milk energy yield was greater with the LFCB diet. The LFCG diet supported the greatest milk, milk protein, and milk energy yield. Decreased concentration of milk protein and increased concentration of milk urea nitrogen when feeding CB compared with CG suggests that lack of fermentable energy in the CB diets may have limited rumen microbial protein synthesis. Total substitution of CG with CB in the nonforage portion did not support maximum milk production, even when forage was reduced at the same time (HFCG vs. LFCB). Predicted neutral detergent fiber (NDF) digestibility at 1 times maintenance, based on chemical analysis of the individual feeds, was 22 percentage units greater for CB than for the forage mix (68.9 vs. 46.9%). In vitro NDF digestibility (30 h) was 19.4 percentage units greater for CB than for the forage mix (68.9 vs. 49.5%). However, in vivo NDF digestibility of the diet when CB replaced forage (HFCB vs. LFCB) was similar (44.1 vs. 44.5%). Similarly, predicted total digestible nutrients at the production level of intake, based on chemical analysis, were greater for the CB treatments and lower for the CG treatments than those observed in vivo.