高效液相色谱法同时测定几类食品中5种添加剂

建立了同时测定几类食品中5种人工合成添加剂(乙酰磺胺酸钾、糖精钠、苯甲酸、山梨酸、脱氢乙酸)的反相高效液相色谱法。样品经前处理后,用VP-ODS-C18(4.6mm×150mm,5μm)柱分离,以0.02mol/L乙酸铵和甲醇(92∶8)为流动相,流速为1.00mL/min,柱温为30℃;使用二极管阵列检测器(DAD)多波长检测,外标法定量。5种添加剂色谱峰分离效果好,在10～100μg/mL浓度范围内呈现良好的线性范围,线性相关系数达到0.999以上,检出限为0.01～0.04μg/mL。平均加标回收率为83.1%～105.7%,相对标准偏差为0.08%～5.24%。该方法法简便、快速、准确,适用于饮料、腌制的蔬菜、蜜饯、发酵豆制品、熟肉制品等食品中5种添加剂的同时检测。     

高效液相色谱法测定饮料中安赛蜜、苯甲酸、山梨酸、糖精钠含量

采用液相色谱条件在波长230nm下，以0．02mol／L乙酸铵：甲醇（95：5）为流动相，快速测定饮料中苯甲酸、山梨酸、糖精钠、安赛蜜含量，样品处理简便快捷。方法添加标准回收率分别为99％、98％、97％、99％。本法与国家标准检验方法（GB／T5009．140—2003、GB／T5009．28—2003、GB／T5009-29—2003）比较，经配对t检验（P〉0．05）无显著性差异。     

Estimation of exposures to non-nutritive sweeteners from consumption of tabletop sweetener products: a review

Reliable estimation of intake of non-nutritive sweeteners (NNS) from tabletop sweetener products (TTS) is complex. Some TTS contain more than one type of NNS and more importantly, there can be considerable formula variation between different types of TTS products; that is liquid, powder and tablet products. A survey of use levels (mg NNS/kg TTS retail product) confirmed wide variations and reflected major differences in the portion size, or mass, typically used to deliver a sweetness equivalent to around one teaspoon (tsp) of sugar. This paper reviews current intake estimation models and reveals that these models may result in inappropriate intake estimations, probably because some surveys did not discriminate between powder, tablet and liquid forms. The data suggest that using upper percentile consumption figures for powdered forms is a critical factor in intake estimations and may be a more realistic method by which overall exposure estimates could be obtained.     

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。     

超高压液相色谱-质谱法测定水果中添加的3种人工合成甜味剂

目的 建立水果中3 种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱 (UPLC-MS/MS)检测方法。方法 以反相C18 柱为色谱柱, 乙腈?0.02 mol/L 乙酸铵溶液为流动相, 样品经纯水 提取后用色谱柱进行分离, 串联质谱负离子多反应监测(MRM)模式测定。结果 3 种人工合成甜味剂在10~600 μg/L 范围内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r≥0.995); 甜蜜素、糖精钠和安赛蜜 的最低检出限分别为0.8、5.0、1.0 μg/kg; 在2 种添加水平下, 样品平均回收率为74.9%~111.2%, 相对标准偏 差<8%。结论 该方法前处理简单, 分析时间短, 具有良好的灵敏度和准确性, 可用于水果中甜蜜素、糖精钠、 安赛蜜的同时检测。     

Longitudinal modelling of the exposure of young UK patients with PKU to acesulfame K and sucralose

ABSTRACT

Artificial sweeteners are used in protein substitutes intended for the dietary management of inborn errors of metabolism (phenylketonuria, PKU) to improve the variety of medical foods available to patients and ensure dietary adherence to the prescribed course of dietary management. These patients can be exposed to artificial sweeteners from the combination of free and prescribed foods. Young children have a higher risk of exceeding acceptable daily intakes (ADI) for additives than adults, due to higher food intakes per kg body weight. Young patients with PKU aged 1–3 years can be exposed to higher levels of artificial sweeteners from these dual sources than normal healthy children and are at a higher risk of exceeding the ADI. Standard intake assessment methods are not adequate to assess the additive exposure of young patients with PKU. The aim of this study was to estimate the combination effect on the intake of artificial sweeteners and the impact of the introduction of new provisions for an artificial sweetener (sucralose, E955) on exposure of PKU patients using a validated probabilistic model. Food consumption data were derived from the food consumption survey data of healthy young children in the United Kingdom from the National Diet and Nutrition Survey (NDNS, 1992–2012). Specially formulated protein substitutes as foods for special medical purposes (FSMPs) were included in the exposure model to replace restricted foods. Inclusion of these protein substitutes is based on recommendations to ensure adequate protein intake in these patients. Exposure assessment results indicated the availability of sucralose for use in FSMPs for PKU leads to changes in intakes in young patients. These data further support the viability of probabilistic modelling as a means to estimate food additive exposure in patients consuming medical nutrition products.     

对安赛蜜生产中回收催化剂工艺的改进

以氨基磺酸、双乙烯酮、三乙胺、三氧化硫、冰醋酸为原料,经乙酰乙酰化、环合、水解、成盐4步反应合成安赛蜜的过程中,会产生一定量的含稀硫酸的溶液。其组分主要为稀硫酸,含有少量三乙胺硫酸盐、丙酮等。生产过程中对三乙胺的回收,对产生的稀硫酸进行中和和对稀酸中约含5%左右的三乙胺硫酸盐回收显得十分重要,这不仅是从经济效益上进行考虑,更是环保要求的需要。通过对安赛蜜生产中回收催化剂工艺进行改进后,不仅能消除碱化解析三乙胺硫酸盐过程中用生石灰粉造成的粉尘污染,又能提高合成安赛蜜过程中三乙胺回收率。     

安赛蜜对大鼠的亚慢性毒性

目的:研究安赛蜜作为食品添加剂的亚慢性毒性。方法:按照GB 15193.13—2015的方法进行亚慢性毒性试验,采用4周龄无特定病原体(SPF)级健康离乳Sprague Dawley (SD)大鼠80只,雌雄各半,设置4个剂量组,分别为阴性对照组和安赛蜜4 500,1 500,500 mg/kg体重3个剂量组,对大鼠进行90 d灌胃染毒,试验结束采血测定血常规及生化指标并进行病理学检测对比。结果:安赛蜜4 500,1 500,500 mg/kg体重3个剂量组动物一般体征正常,试验末期体重增长量、总摄食量、总食物利用率以及绝对脏器重量、脏体比未发现有意义的异常改变;血液学检测值、生化指标检测值、尿液指标值均在正常波动范围内,与对照组比较差异无统计学意义(P>0.05)。动物大体检查未发现心、肝、脾、肺、肾、睾丸、心脏、胸腺和肾上腺等脏器的异常改变,组织病理学镜检未发现与受试物相关的病理改变。结论:安赛蜜在整个试验周期对大鼠均未见明显的毒性作用,90 d经口未观察到有害作用剂量为4 500 mg/kg体重。     

湖北省食品中甜蜜素和安赛蜜的风险评估

目的 为对湖北省食品中添加剂进行风险分析,为相关部门制定管理措施提供依据,降低食品安全潜在的危害因素及概率.方法 本文主要运用水晶球软件,应用蒙特卡洛模拟法,对湖北省食品中甜蜜素和安赛蜜的每日平均暴露量和风险概率进行评估.结果 腌菜制品中甜蜜素的每日平均暴露量和风险熵最高,分别为3.98E-4 g/kg·BW·d和0....     

苹果醋中安赛蜜、山梨酸和日落黄成分分析标准物质的研制

研制了苹果醋中安赛蜜、山梨酸和日落黄成分分析标准物质,优化并建立了高效液相色谱-二极管阵列检测器（HPLC-DAD）方法对目标物分析测量。标准物质的均匀性经单因素方差分析显示均匀,稳定性经线性回归趋势分析表明在7个月内量值稳定。定值方式采用多家实验室（9家）合作定值。 标准值及扩展不确定度(k=2):安赛蜜(141±8)mg/kg, 山梨酸(259±12)mg/kg, 日落黄(8.45±0.33)mg/kg。