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。     

Estimated intake of the sweeteners,acesulfame-K and aspartame,from soft drinks,soft drinks based on mineral waters and nectars for a group of Portuguese teenage students

In a survey of levels of acesulfame-K and aspartame in soft drinks and in light nectars, the intake of these intense sweeteners was estimated for a group of teenage students. Acesulfame-K was detected in 72% of the soft drinks, with a mean concentration of 72 mg l^?1 and aspartame was found in 92% of the samples with a mean concentration of 89 mg l^?1. When data on the content of these sweeteners in soft drinks were analysed according to flavour, cola drinks had the highest mean levels for both sweeteners with 98 and 103 mg l^?1 for acesulfame-K and aspartame, respectively. For soft drinks based on mineral water, aspartame was found in 62% of the samples, with a mean concentration of 82 mg l^?1 and acesulfame-K was found in 77%, with a mean level of 48 mg l^?1. All samples of nectars contained acesulfame-K, with a mean concentration of 128 mg l^?1 and aspartame was detected in 80% of the samples with a mean concentration of 73 mg l^?1. A frequency questionnaire, designed to identify adolescents having high consumption of these drinks, was completed by a randomly selected sample of teenagers (n = 65) living in the city of Coimbra, in 2007. The estimated daily intakes (EDI) of acesulfame-K and aspartame for the average consumer were below the acceptable daily intakes (ADIs). For acesulfame-K, the EDI was 0.7 mg kg^?1 bw day^?1 for soft drinks, 0.2 mg kg^?1 bw day^?1 for soft drinks based on mineral waters, and 0.5 mg kg^?1 bw day^?1 for nectars, representing 8.0%, 2.2%, and 5.8% of the ADI, respectively. A similar situation was observed for aspartame. In this way, the EDI for soft drinks was 1.1 mg kg^?1 day^?1, representing only 2.9% of the ADI. In respect of nectars, the EDI was 0.2 mg kg^?1 bw day^?1, representing 0.5% of the ADI. Soft drinks based on mineral waters showed the lowest EDI values of 0.3 mg kg^?1 bw day^?1, accounting for 0.7% of the ADI.     

饮料及果品中糖精、苯甲酸、山梨酸和咖啡因的反相HPLC同时快速测定

用SUPELCOSIL LC－8－DB柱为分离柱（柱温30℃）、以30：70（体积比）的甲醇：草酸铵溶液（1.25g/L)作流动相,在230nm紫外检测,反相HPLC同时快速测定了饮料和果品中的糖精、苯甲酸、山梨酸和咖啡因四种食品添加剂。在试验浓度范围2－200mg/L内均呈良好线性,它们的检出限分别为20、8、2、26ng。样品的加标回收率为104％－112％,变异系数为2．5％－4．6％（n=5）。     

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。     

江西省居民膳食中山梨酸及其钾盐暴露风险评估

目的评估江西省居民膳食中山梨酸及其钾盐的暴露水平和潜在健康风险。方法利用2012—2016年江西省食品中山梨酸及其钾盐含量数据、2016年江西省居民食物消费量调查数据,采用简单分布评估法计算江西省居民膳食中山梨酸及其钾盐的暴露水平,并进行健康风险评估。结果江西省居民膳食中山梨酸及其钾盐每日平均暴露量及每日高暴露量(P95)分别为0.031和0.085 mg/kg BW,分别占暂定组每日允许摄入量(ADI,3 mg/kg BW)的1.03%和2.83%。西式糕点、大米制品、熟肉制品是江西省居民膳食中山梨酸及其钾盐暴露的主要来源,贡献率达到总膳食暴露量的75%以上。如果严格执行GB 2760—2014《食品安全国家标准食品添加剂使用标准》中关于山梨酸及其钾盐限量规定,江西省居民膳食中山梨酸及其钾盐每日平均暴露量和每日高暴露量分别下降25.7%～49.5%和14.5%～27.9%,西式糕点、果蔬汁类饮料、新型豆制品则成为膳食中山梨酸及其钾盐暴露的主要来源。结论目前江西省居民膳食中山梨酸及其钾盐暴露量对人群健康造成的风险较低,处于可接受水平,但仍有部分暴露来源于食品添加剂滥用,需要关注。     

离子对色谱法测定含乳饮料中糖精钠、苯甲酸和山梨酸的含量

采用离子对色谱法．在Zorbax Eclipse XDB-C8柱上．以甲醇；水(38：62)内含0．02M的HAc-NaAc和0．005M的四丁基溴化饺作流动相，紫外230nm检测．快速测定含乳饮料中的糖精钠、苯甲酸和山梨酸的三种食品添加剂吉量．在试验浓度范围5-200mg／L内均呈良好线性．三种添加剂的检测限分别为5ng、4ng、4ng．样品的加标回收率为98．0％～107％．方法的相对标准偏差小于2．2％。     

A screening method for the determination of ascorbic acid in fruit juices and soft drinks

A simple and rapid liquid chromatographic method based on a new stationary phase Teknokroma, Tr-010065 Mediterranea sea₁₈ (15 cm × 0.4 cm, id 3 μm), to determine ascorbic acid in beverages is reported. With the proposed method the samples were analysed by direct injection without a previous treatment. The total analysis time does not exceed 6 min. The method showed a good repeatability (RSD < 2%: n = 6) and an excellent sensitivity (LOD = 0.01 mg/l). Seventeen samples were analysed, including fruit juices, soft drinks and isotonic beverages. Ascorbic acid contents ranged from 6.6 to 840 mg/l. The ascorbic acid stability in some beverages during their shelf-life was also evaluated. Degradation of about 54% was observed in a tea drink.     

高效液相色谱法测定黄酒中苯甲酸、山梨酸和糖精钠含量

目的建立高效液相色谱法测定黄酒中苯甲酸、山梨酸和糖精钠的分析方法。方法样品经称取、加热、定容,利用高效液相色谱法检测,甲醇水混合溶液作为流动相,PDA检测器检测,苯甲酸、山梨酸和糖精钠的检测波长为230nm。结果苯甲酸和山梨酸在0.05~0.30 mg/mL、糖精钠在0.0025~0.0125mg/mL时,都具有良好的线性关系,相关系数(r)均0.999。苯甲酸、山梨酸和糖精钠的LOD分别为1.8、1.2、0.1g/kg,LOQ分别为5.4、3.6、0.3mg/kg。平均加标回收率为95.1%~96.4%,RSD为2.6%~3.8%。50份黄酒样品中,苯甲酸检出有19份,检出率为38.0%,检测结果范围为0.0025~1.48g/kg;山梨酸检出有6份,检出率为12.0%,检测结果范围为0.028~0.44g/kg;糖精钠检出有24份,检出率为48.0%,检测结果范围为0.005~0.73g/kg。结论该方法灵敏度高,回收率高,检测限低,符合分析要求,适合黄酒中苯甲酸、山梨酸和糖精钠的检测要求。     

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。     

2018年湖北省食品中苯甲酸、山梨酸、糖精钠的抽检结果分析

目的 了解湖北省食品中苯甲酸、山梨酸、糖精钠的使用安全状况, 为省食品安全监管工作提供科学依据。方法 对2018年各类食品按照相关标准进行检验和评价, 对检测结果进行分析。结果 2018年共检测食品887批次, 总合格率为94.25%。苯甲酸、山梨酸超标使用的情况分布在水果制品、豆制品和餐饮食品中。结论 2018年湖北省食品安全状况总体良好, 但也存在一些问题。相关部门应加大对小作坊的监督力度, 规范生产, 保障消费者的身体健康。     

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.     

武汉市热干面散装调料中苯甲酸、山梨酸、糖精钠监测结果分析

目的调查武汉市小型餐饮单位热干面调料中苯甲酸、山梨酸和糖精钠含量情况,并对监测结果进行分析。方法根据随机抽样法采集武汉市小型餐饮单位热干面调料共251件,采用高效液相色谱法检测其中苯甲酸、山梨酸和糖精钠的含量。结果 251件热干面调料中苯甲酸、山梨酸和糖精钠均有检出和超标,总检出率为72.9%,总超标率为26.7%,4类不同样品中3种食品添加剂检出率存在显著性差异(P0.05);中心城区和新城区热干面调料中3种添加剂超标率无显著性差异。结论武汉市小型餐饮单位热干面调料中苯甲酸、山梨酸和糖精钠存在超限量滥用现象,相关部门需要加大对该类食品中3类食品添加剂查处力度。     

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。     

Exposure assessment of food preservatives (sulphites,benzoic and sorbic acid) in Austria

An exposure assessment was performed to estimate the potential intake of preservatives in the Austrian population. Food consumption data of different population groups, such as preschool children aged 3–6 years, female and male adults aged 19–65 years were used for calculation. Levels of the preservatives in food were derived from analyses conducted from January 2007 to August 2010. Dietary intakes of the preservatives were estimated and compared to the respective acceptable daily intakes (ADIs). In the average-intake scenario, assuming that consumers randomly consume food products that do or do not contain food additives, estimated dietary intakes of all studied preservatives are well below the ADI for all population groups. Sulphite exposure accounted for 34%, 84% and 89% of the ADI in preschool children, females and males, respectively. The mean estimated daily intake of benzoic acid was 32% (preschool children), 31% (males) and 36% (females) of the ADI. Sorbic acid intakes correspond to 7% of the ADI in preschool children and 6% of the ADI in adults. In the high-intake scenario assuming that consumers always consume food products that contain additives and considering a kind of brand loyalty of consumers, the ADI is exceeded for sulphites among adults (119 and 124%, respectively). Major contributors to the total intake of sulphites were wine and dried fruits for adults. Mean estimated dietary intakes of benzoic acid exceeded the ADI in all population groups, 135% in preschool children, 124% in females and 118% of the ADI in males, respectively. Dietary intakes of sorbic acid are well below the ADI, accounting for a maximum of 30% of the ADI in preschool children. The highest contributors to benzoic and sorbic acid exposure were fish and fish products mainly caused by high consumption data of this large food group, including also mayonnaise-containing fish salads. Other important sources of sorbic acid were bread, buns and toast bread and fruit and vegetable juices.     

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。     

黄酒中苯甲酸本底含量与溯源分析及初步风险评估

目的对黄酒中苯甲酸的本底含量进行调查与溯源分析,并对我国居民成年饮黄酒者的苯甲酸摄入量进行评估以了解其健康风险。方法从山东省、浙江省、江苏省、福建省、上海市等我国主要五大黄酒产区采集黄酒样品231份及其加工原料15份,并采用液相色谱法对其中苯甲酸及其前体物质的含量进行测定;采用苯甲醛和苯丙氨酸模拟试验以及实际样品加速试验对黄酒中苯甲酸的来源进行溯源分析;并采用简单分布评估方法对我国居民成年饮黄酒者的苯甲酸摄入量进行评估。结果黄酒中苯甲酸检出率为99.13%(229/231),含量范围为ND(未检出)～37.00 mg/L,均值为2.28 mg/L。其中,98份成品酒中,苯甲酸检出率为100.00%(98/98),含量范围为ND～1.60 mg/L,均值为0.52 mg/L;133份基础酒中,苯甲酸检出率为98.50%(131/133),含量范围为ND～37.00 mg/L,均值为3.58 mg/L。溯源分析结果显示,黄酒中苯甲酸主要来自加工原料带入、苯丙氨酸降解以及苯甲醛氧化生成。暴露评估结果显示,我国黄酒消费人群苯甲酸的平均暴露量为0.001 mg/kg BW,占每日允许摄入量(ADI)的0.02%;P95暴露量为0.005 mg/kg BW,占ADI的0.1%。结论黄酒中苯甲酸的检出率高但本底含量较低,其主要来源为加工原料带入、苯丙氨酸降解以及苯甲醛氧化生成;我国居民成年饮黄酒者的苯甲酸的暴露风险较低。     

Occurrence and dietary exposure assessment of multiple mycotoxins in corn-based food products from Shandong,China

This study was designed to investigate the occurrence and exposure assessment of multiple mycotoxins in corn-based food products from Shandong Province, China. Results demonstrated that the mean level of total mycotoxins in test samples was 197.2 µg/kg. The most frequently found mycotoxins were deoxynivalenol (96.7%) and fumonisin B₁ (94.4%), with mean contamination levels of 65.24 and 128.2, respectively. Among these corn-based food products, thin corn pancake had the highest mean contamination (886.7 µg/kg), followed by wotou (143.7 µg/kg), corn cake (135.4 µg/kg) and mantou (63.73 µg/kg). The average exposure values to total fumonisins and deoxynivalenol were 0.05 and 0.02 µg/kg bw/day, which were lower than the provisional maximum tolerable daily intake values of 2 and 1 µg/kg bw/day, respectively, as established by the Joint FAO/WHO Expert Committee on Food Additives. In the future strict control and systematic monitoring are needed to secure food safety and human health.