同位素稀释-超高效液相色谱-串联质谱法同时测定婴幼儿谷类辅助食品中的15种真菌毒素和6种农药残留

目的 建立了同位素稀释-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS) 同时测定婴幼儿谷类辅助食品中15种真菌毒素和6种农药残留的方法。方法 样品经乙腈-水-甲酸(84:15:184∶15∶1, V:/V:V )提取并低温高速离心后, 直接用水稀释提取液, 加入同位素内标消除基质效应影响, 以BEH C18为分离柱, 利用UPLC-MS/MS测定, 在多反应监测模式下内标法定量。结果 在最佳实验条件下, 目标物在各自线性范围内线性良好, 相关系数(r)均大于0.999; 检出限为0.03~7 μg/kg0.03 μg/Kg~7 μg/Kg , 定量限为0.1~20 μg/kg 0.1 μg/Kg~20 μg/Kg; 加标回收率在75%~108%之间, 相对标准偏差(RSD)为2.8%~11%。结论 该方法前处理简单快速、灵敏度高、准确性好,有效解决基质效应问题,适用于大批量婴幼儿谷类辅助食品中15种真菌毒素和6种农药残留的同时测定。     

婴幼儿谷类辅助食品中脱氧雪腐镰刀菌烯醇污染水平及其风险评估

目的 了解我国市售婴幼儿谷类辅助食品(以下简称谷类辅食)脱氧雪腐镰刀菌烯醇(DON)污染情况并评估婴幼儿来源于谷类辅食的DON暴露风险。方法 在我国6省共采集了360份市售谷类辅食样品,包括米粉类183份、饼干类91份、面条类67份、其他类19份,检测每份样品中DON、3-乙酰脱氧雪腐镰刀菌烯醇(3-Ac-DON)和15-乙酰脱氧雪腐镰刀菌烯醇(15-Ac-DON)含量。分别采用点评估和简单分布评估方法估计3岁以下婴幼儿来源于谷类辅食的DON急性和慢性暴露风险。结果 谷类辅食DON检出率为60.3%(217/360),平均含量为116.3 μg/kg,最大值为1 198.7 μg/kg;面条类DON平均含量最高(342.7 μg/kg),其次为饼干类(173.0 μg/kg),米粉类最低(12.0 μg/kg)。3岁以下婴幼儿食用面条类辅食的DON急性暴露量可能超过成组急性参考剂量(ARfD)。食用谷类辅食的婴幼儿DON平均暴露量为0.27 μg/(kg·d),其中7.3%(243/3 320)的个体来源于谷类辅食的DON暴露量超过成组暂定每日最大耐受摄入量。不同年龄组谷类辅食食用者DON平均暴露量分别为0～<1岁0.22 μg/(kg·d)、1～<2岁0.31 μg/(kg·d)、2～<3岁0.37 μg/(kg·d)。面条类辅食对DON平均暴露量的贡献率最高,达77.8%。结论 在当前谷类辅食DON污染水平下,3岁以下婴幼儿来源于谷类辅食的DON暴露量可能存在健康风险,需要关注。     

我国市售婴幼儿谷类辅助食品营养成分含量水平研究

了解我国市售婴幼儿谷类辅助食品营养成分含量水平,为GB 10769-2010《食品安全国家标准 婴幼儿谷类辅助食品》标准修订提供参考。收集我国市售婴幼儿谷物辅助食品、婴幼儿高蛋白谷物辅助食品、婴幼儿生制类谷物辅助食品和婴幼儿饼干类辅助食品,对GB 10769-2010中规定的基本营养成分和可选择营养成分含量进行检测,对检测结果进行统计分析。共收集婴幼儿谷类2004份,其中婴幼儿谷物辅助食品1850份,婴幼儿高蛋白辅助食品50份,婴幼儿生制类食品51份,婴幼儿饼干53份。婴幼儿高蛋白谷物辅助食品蛋白质平均含量高于其他3类谷物辅助食品蛋白质含量,为0.88 g/100 kJ,差异具有统计学意义(P<0.05)。婴幼儿饼干类辅助食品能量和脂肪平均含量高于其他3类谷物辅助食品能量和脂肪含量,分别为1777 kJ/100 g和0.55 g/100 kJ,差异具有统计学意义(P<0.05)。GB 10769-2010有下限值和上限值范围值的营养素,维生素A、维生素D、钙、铁、锌、维生素E、磷、碘、钾等含量平均值分别接近各自理论平均值。GB 10769-2010无上限值范围值的营养素,市售产品其含量范围的最大值是国标下限值的2.83~67.04,其含量范围的95百分位数是国标下限值的2.05~16.35。GB 10769-2010中未制定上限值的营养成分出现离群值。建议综合考虑我国市售婴幼儿谷类辅助食品营养素含量分布情况,对无上限值的营养素进行修订。     

《婴幼儿谷类辅助食品》(GB 10769—2010)跟踪评估研究

目的 了解我国监督部门、检验机构和生产企业对GB 10769-2010《婴幼儿谷类辅助食品》的依从性和贯彻实施情况,以期为今后标准的制修订提供资料.方法 通过现况调查,了解婴幼儿谷类辅助食品主产区的监管部门、检验机构和生产企业的基本情况、对标准条款的理解、各项指标的检测能力和标准的实施情况,收集标准执行过程中遇到的主要问题以及反馈的意见和建议.结果 向监督部门、检验机构和生产企业分别发放问卷176、90和56份,有效问卷回收率分别为95.5％、91.1％和85.7％,不同部门均认为标准的整体合理程度较高(89.3％、90.2％、95.9％),收集的反馈意见分别为235、231和207条,大型、外资企业和监督部门、检验机构中从事食品监管和检验工作时间较长以及标准使用频率较高、积极参加各项培训活动的人员反馈问题相对较多.其中产品分类、原料要求、基本营养成分、污染物和真菌毒素限量部分的反馈意见相对集中.结论 通过跟踪调查发现标准整体合理程度较高,部分指标需要跟进新的风险评估结果并及时更新指标值,某些重点营养素亟需出台配套的国标检验方法.加大监管部门、中小企业标准培训的力度和深度,并发挥媒体在标准宣贯中的积极作用,对各方正确执行标准有重要意义.     

婴幼儿谷类辅助食品加工工艺对其脱氧雪腐镰刀菌烯醇及衍生物影响

脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)是由镰刀菌在侵染小麦等禾谷类作物过程中产生的一种有毒次级代谢产物,主要污染小麦、大麦、燕麦、黑麦和玉米等谷物。DON在植物和微生物作用下会转化形成各种衍生物,且这些衍生物可与DON原型同时存在,增加了谷物及其相关制品的安全风险。谷类辅食是婴幼儿膳食中的重要组成部分,且婴幼儿对毒素的敏感性更强,应严格限制DON及其衍生物在谷类辅食中被检出。已有研究表明谷物类食品的制作加工方式会对DON及其衍生物的含量水平产生影响,但专门针对婴幼儿消费人群的谷类辅助食品的加工过程如何影响DON及其衍生物水平还鲜有报道。目前婴幼儿谷类辅助食品中DON及其衍生物含量存在超标问题,严重影响婴幼儿这类特殊人群的生长发育和健康。本文从婴幼儿谷类辅食中DON及其衍生物的污染状况及其在加工过程中的含量变化等方面进行较为详细的阐述,以期为婴幼儿谷类辅食中DON的风险评估及防控策略的制定提供有利参考。     

2015~2019年度婴幼儿谷类辅助食品监督抽检结果统计与分析

目的 分析2015~2019年度婴幼儿谷类辅助食品安全整体状况,了解不合格主要指标。方法 从国家市场监督管理总局网站收集2015~2019年度婴幼儿谷类辅助食品监督抽检公告资料,对抽检结果进行统计与分析;合格率的比较采用卡方检验分析。结果 从2015～2019年度4月上旬,共抽检样品1773批次,合格率为92.39%。2015年抽检合格率最低为89.50%,其他年度抽检合理率均高于93%。中国大陆婴幼儿谷类辅助食品生产企业的产品抽检合格率为92.83%,高于其他食品生产企业的合格率87.23%。不合格项目主要为维生素类指标和钠。结论 我国市售婴幼儿谷类辅助食品合格率较高,总体呈平稳向好趋势。     

Evaluation of enniatins A,A1, B,B1 and beauvericin in Portuguese cereal-based foods

Sixty-one samples of Portuguese cereal-based foods were analysed for the occurrence of emerging mycotoxins called enniatins (A, A1, B and B1) and beauvericin. Samples were extracted with a mixture of acetonitrile/water (85/15, v/v) using an Ultra-Turrax homogeniser, and mycotoxins were detected with liquid chromatography coupled to a mass spectrometer. This method was validated and adequate values of recovery (70–103%) and relative standard deviation (<15%) were obtained. Signal suppression/enhancement was studied and matrix-matched calibration used to minimise this effect, but no additional clean-up step was necessary. The mass spectrometer was operated in selected reaction monitoring (SRM) mode and with selected transitions for each compound to quantify and to qualify them. Fifty-nine per cent of samples were contaminated. The percentages of enniatins were 53%, 49%, 44% and 16% for A1, B, B1, and A, respectively, and for beauvericin it was 1.6%. For the total samples, the mean contamination was 30, 24, 15, 2.1 and 0.1?ng?g^?1 for enniatins A1, B, B1 and A, and beauvericin, respectively. The wheat-based samples showed higher levels and greater prevalence than any other cereals monitored. These results were used to estimate the daily intake of ENs from wheat-based cereal by the Portuguese population. At the same time, the usefulness of this method in the analysis of other important mycotoxins (aflatoxin B₁, ochratoxin A, deoxynivalenol, T-2 toxin, fumonisin B₁ and zearalenone) was evaluated.     

我国市售婴幼儿谷类辅助食品可选择营养成分使用现况调查

目的:了解我国市售婴幼儿谷类辅助食品可选择营养成分添加情况和含量分布,为修订《婴幼儿谷类辅助食品》(GB10769-2010)可选择营养成分提供参考依据。方法:通过线下实体店和网店收集婴幼儿谷类辅助食品标签信息,将产品信息及可选择营养成分录入Excel表格,用SPSS 21.0统计各可选择营养成分添加率及含量分布,用秩和检验比较不同类别谷物辅助食品含量差异。结果:55家企业的247例婴幼儿谷类辅助食品纳入分析。现行标准中规定的所有可选择营养成分均有使用,不同类型的婴幼儿谷物辅助食品添加的可选择营养成分不同。各可选择营养成分含量整体处于标准范围值的较低区间。维生素B_2和烟酸添加率最高,分别为70.8%和70.0%;添加率最高的矿物质磷为54.2%,添加率最低的酪蛋白磷酸肽为3.6%。婴幼儿高蛋白辅助食品中的维生素E、维生素B_6、维生素B_(12)、泛酸、维生素C和磷含量高于其他3类婴幼儿谷物食品中的含量,差异具有统计学意义(P 0.05)。结论《婴幼儿谷类辅助食品》(GB10769-2010)规定的可选择营养成分均有使用,不同类型的婴幼儿谷物辅助食品添加的可选择营养成分不同。各可选择营养成分含量总体处在标准范围值的低区间。     

0～36月龄婴幼儿配方食品及婴幼儿辅助食品中糖含量分析

目的 了解我国市售婴幼儿配方食品（婴儿配方食品、较大婴儿配方食品和幼儿配方食品）及婴幼儿辅助食品（婴幼儿谷类辅助食品和罐装辅助食品）中葡萄糖、半乳糖、果糖、乳糖、蔗糖和麦芽糖的含量,为婴幼儿配方食品及婴幼儿辅助食品相关的食品安全标准管理提供数据支持。方法 根据随机抽样原则,采集国内市场常见的婴幼儿配方食品及婴幼儿辅助食品83例,涵盖婴幼儿配方食品、婴幼儿谷类辅助食品和婴幼儿罐装食品等,利用离子色谱-脉冲安培法对葡萄糖、半乳糖、果糖、乳糖、蔗糖和麦芽糖进行含量检测,并对检测结果进行分析。结果 婴幼儿配方食品中总糖含量的中位数为433.43～476.99 g/kg,其中乳糖占总糖的比均高于95%,乳糖含量由高至低分别为婴儿配方食品、较大婴儿配方食品和幼儿配方食品。婴幼儿谷类辅助食品中总糖检出率为36.8%,含量中位数为0～28.35 g/kg,其乳糖和蔗糖的中位数较高,为84.30和70.17 g/kg,而蔗糖在饼干第三四分位数（Q3）的含量较高,为53.43 g/kg。国产和原装进口配方食品的添加糖含量进行比对,差异没有统计学意义（P>0.05）。结论 我国市售的婴幼儿配方食品中乳...     

Co-occurrence of mycotoxins in commercial formula milk and cereal-based baby food on the Qatar market

The present study was conducted to explore the occurrence of mycotoxins in commercial baby foods in Doha-Qatar. LCMS/MS- and HPLC-based analysis of baby food (n = 67) for 12 mycotoxins confirmed the presence of aflatoxin M1 (AFM1, 33%), ochratoxin A (OTA, 31%), deoxynivalenol (DON, 27%), aflatoxin B1 (AFB1, 22%), fumonisin B2 (FB2, 10%), zearalenone (ZEN, 4%) and T-2 toxin (2%). Noodles exhibited the maximum contamination percentage, with 33% of the samples being contaminated above the EU maximum limits, for at least one mycotoxin. Among the multi-grain flake samples, up to 28% and for the milk and milk-based-cereal samples, 14% contained at least one mycotoxin above the EU maximum limits. From all cereal-based food samples, 22%, 5%, 2% and 2% were concurrently contaminated with 2, 3, 4 and 5 mycotoxins, respectively. The occurrence of toxicological important mycotoxins in Qatari market warrants the implementation of strict regulatory limits to protect human health.     

2018年河南省市售婴幼儿谷类辅助食品微生物污染状况调查

目的 了解河南省市售婴幼儿谷类辅助食品卫生状况,为食品安全风险评估及标准制定提供基础数据。方法 参照《2018年国家食品污染物和有害因素风险监测工作手册》提供方法进行采样和检测,在河南省共采集婴幼儿谷类辅助食品103份,对其进行肠杆菌科、蜡样芽胞杆菌、单核细胞增生李斯特菌和克罗诺杆菌属污染状况检测,对检测中可疑菌落采用基质辅助激光解吸电离飞行时间质谱进行鉴定。结果 103份样品中肠杆菌科和克罗诺杆菌属检出率分别为0.97%(1/103)和5.83%(6/103),均在婴幼儿即食谷物辅助食品中检出,产地集中在江西省和福建省,采样地点类型均为便利店/零售店,6份克罗诺杆菌属阳性样品中有5份样品标识为≥辅食添加初期。9份样品蜡样芽胞杆菌定量结果在10～10³ CFU/g范围,检出率为8.74%(9/103),样品产地包括广东省、江西省、福建省、黑龙江省和四川省,采样地点类型均为超市和便利店/零售店,其中有8份是婴幼儿即食谷物辅助食品。结论 河南省市售婴幼儿谷类辅助食品尤其是婴幼儿即食谷物辅助食品受到克罗诺杆菌属和蜡样芽胞杆菌污染,且这些阳性产品中大多数标识的适用年龄为≥辅食添加初期,由此带来的食品安全风险较大,建议婴幼儿即食谷物辅助食品添加克罗诺杆菌属和蜡样芽胞杆菌微生物限量,降低由此带来的食品安全隐患。     

浅析婴幼儿食品中食品添加剂的使用管理问题

婴幼儿食品安全是食品安全工作的重点领域。目前,婴幼儿食品中违规使用非食用物质和滥用食品添加剂的现象依然存在。为建立合理的添加原则,保障产品的质量,减少因滥用食品添加剂所致的健康危害,国际组织和我国均制定了相应的法规和标准。本文全面系统地介绍了国际和国内涉及婴幼儿食品中食品添加剂使用的相关法规和标准概况,并对我国婴幼儿食品中食品添加剂的使用安全问题进行了分析,旨在对我国婴幼儿食品中食品添加剂的使用管理提供参考和借鉴。     

实时荧光PCR法测定婴幼儿辅助食品中过敏原鱼类成分

目的建立实时荧光PCR检法测定婴幼儿辅助食品中过敏原鱼类成分。方法通过改进的前处理方法,采用实时荧光PCR法,对45个样品进行检测,分别进行特异性、检出限以及适用性试验。结果用于特异性试验的18个样品中,只有鱼类出现特异性扩增;通过7个不同质量配比的鱼肉样品得出检出限低于0.01%;对市售20批样品进行检测,检测结果与样品标识相符。结论该方法快速、灵敏、准确,适用于婴幼儿辅助食品中过敏原鱼成分的检测。     

婴幼儿配方食品和乳粉中维生素C的测定

目的建立一种前处理简单、仪器条件稳定、准确高效的婴幼儿配方食品和乳粉中维生素C的检测方法。方法用含有三(2-羧乙基)膦(TCEP)的三氯乙酸(TCA)对样品中的维生素C进行提取,C18柱色谱分离,流动相为含TCEP与癸胺作为离子对试剂和pH 5.4的醋酸钠的混合水溶液,然后在紫外检测器265 nm处进行检测。结果本方法的相对标准偏差(n=6)在0.36%~3.2%之间,平均回收率为88.5%~97.9%,线性相关系数r~2大于0.9999。结论本方法实验前处理简单,干扰因素少;仪器条件稳定,灵敏度高,重复性好;适合婴幼儿配方食品和乳粉复杂基质样品的测定。     

Extraction and reliable determination of acrylamide from thermally processed foods using ionic liquid-based ultrasound-assisted selective microextraction combined with spectrophotometry

Acrylamide (AAm) is a carcinogenic chemical that can form in thermally processed foods by the Maillard reaction of glucose with asparagine. AAm can easily be formed especially in frequently consumed chips and cereal-based foods depending on processing conditions. Considering these properties of AAm, a new, simple and green method is proposed for the extraction of AAm from thermally processed food samples. In this study, an ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, [Bmim][BF₄]) as extractant was used in the presence of a cationic phenazine group dye, 3,7-diamino-5-phenylphenazinium chloride (PSH⁺, phenosafranine) at pH 7.5 for the extraction of AAm as an ion-pair complex from selected samples. Under optimum conditions, the analytical features obtained for the proposed method were as follows; linear working range, the limits of detection (LOD, 3S_b/m) and quantification (LOQ, 10S_b/m), preconcentration factor, sensitivity enhancement factor, sample volume and recovery% were 2.2–350 µg kg^?1, 0.7 µg kg^?1, 2.3 µg kg^?1, 120, 95, 60 mL and 94.1–102.7%, respectively. The validity of the method was tested by analysis of two certified reference materials (CRMs) and intra-day and inter-day precision studies. Finally, the method was successfully applied to the determination of AAm levels in thermally processed foods using the standard addition method.     

Selecting desirable micronutrient fortificants for plant‐based complementary foods for infants and young children in low‐income countries

The World Health Organization (WHO) recommends that both breast‐fed and non‐breast‐fed children are fed micronutrient fortified complementary foods designed to meet their high nutrient requirements from aged 6 to 23 months of age. This paper summarises the steps recommended by WHO/FAO to identify the country‐specific micronutrient shortfalls in complementary diets and establish desirable levels of bioavailable fortificants for centrally processed plant‐based complementary foods for infant and young child feeding. The goal of the WHO/FAO guidelines is to achieve a desirably low prevalence of inadequate micronutrient intakes in the target group whilst simultaneously ensuring minimal risk of excessive intakes. © 2014 Society of Chemical Industry     

Occurrence of emerging mycotoxins in cereals and cereal-based products from the Korean market using LC-MS/MS

The present study aimed to investigate the occurrence of emerging mycotoxins in cereals (n = 61) and cereal-based products (n = 36) collected from Korean market. First of all, using the quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction method, and ultrahigh-pressure liquid chromatography (UPLC) with triple quadruple tandem mass spectrometry (MS/MS), we developed a simple and fast method for quantitative determination of eight emerging mycotoxins including alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), beauvericin (BEA) and enniatins (ENs; ENA, ENA1, ENB and ENB1). The developed analytical method was validated in parameters of linearity, precision and accuracy. For UPLC-MS/MS analysis, the recoveries of emerging mycotoxins from spiked samples at three concentration levels ranged from 82.7% to 108.8% with RSDs between 0.4% and 14.7%. Analytical methods were applied to determine the contamination of mycotoxins in cereal and cereal-based product samples. Sixty-three of the total 97 samples were contaminated with at least one emerging mycotoxin. The maximum number of emerging mycotoxins observed in a single sample was six out of eight analytes. The highest level of contamination was detected in cereal at 70.9 μg/kg for alternariol monomethyl ether (AME). However, currently there is no international standard for emerging mycotoxins in food. Accordingly, it is necessary to establish a database of emerging mycotoxins contamination through continuous monitoring.     

市售婴幼儿食品中克罗诺杆菌分离菌株脉冲场凝胶电泳分型及耐药性研究

目的研究婴幼儿食品中克罗诺杆菌分离菌株的分子分型特征和耐药情况。方法 2010—2016年在国内32个企业生产的婴幼儿食品中分离获得50株克罗诺杆菌,使用限制性内切酶XbaⅠ对基因组DNA进行酶切和脉冲场凝胶电泳(PFGE)分型,利用BioNumerics软件进行聚类分析,采用微量肉汤稀释法进行药敏试验,分析分离菌株的耐药情况。结果 50株克罗诺杆菌分为47个PFGE型,相似度为28.7%～100.0%,具有较高的遗传多态性。不同地区、不同企业的分离株分散在各簇,无地区聚集性和特异性,但有2个企业不同批次产品的分离菌株分别属于同一克隆株。50株克罗诺杆菌对萘啶酸、环丙沙星、头孢吡肟、阿米卡星、头孢噻肟和头孢曲松均敏感,对磺胺嘧啶、氨苄青霉素、氯霉素、复方新诺明、阿莫西林-克拉维酸、卡那霉素和庆大霉素具有不同程度的耐药,7株克罗诺杆菌表现出对抗生素的多重耐药性。结论部分婴幼儿食品加工企业存在克罗诺杆菌持续污染,且有多重耐药株出现,应加强关注。