婴幼儿配方奶粉中邻苯二甲酸酯的固相萃取净化-气相色谱-质谱法测定

建立婴幼儿配方奶粉中邻苯二甲酸酯(PAEs)固相萃取净化,气相色谱-质谱法测定的方法。样品加入同位素内标后,以乙腈提取,PSA/Silica固相萃取柱净化,气相色谱-质谱法检测,内标法定量。结果表明:该方法对婴幼儿配方奶粉的16种PAEs定量限为50~100μg/kg,加标回收率在74%~124%之间,RSD在0.78%~7.1%之间。该方法简便快捷,定量准确,重现性好,适用于高通量检测婴幼儿配方奶粉中PAEs质量分数。     

毛细管气相色谱法测定婴幼儿配方乳粉中碘的质量

婴幼儿配方奶粉中碘的测定方法存在重现性差,样品处理繁琐等问题。本文建立了毛细管柱气相色谱仪快速测定婴幼儿配方乳粉中碘的方法。结果表明,在1.0~10.0μg范围内,碘的峰面积与其质量呈良好的线性关系,相关系数r为0.9995,方法的最低检出限(S=3N)为1.5μg/100g,3个添加水平(1,4和8μg)的平均回收率为87.2%~105.2%,相对标准偏差(RSD)为3.1%~5.2%。该方法操作简便、快速、准确,减少了复杂的前处理环节,能够满足婴幼儿配方奶粉中碘质量的测定。     

婴幼儿配方乳粉中微量碘测定方法的比较

本文采用气相色谱法(GC)、电感耦合等离子体质谱法(ICP-MS)、离子色谱法(IC)分别测定了婴幼儿配方乳粉中碘的含量。通过多方面因素对比:前处理的方式、碘的测定种类、方法线性范围、回收率、检出限、精密度等,得出电感耦合等离子体质谱法前处理操作简便,受奶粉复杂基质干扰最小,在1~50μg/L线性范围内,相关系数可达到0.999以上。回收率在95.9%~103.7%之间,RSD为0.6%~2.2%,检出限为0.6μg/100g,最适合用于婴幼儿配方乳粉中微量碘的实验室常规分析。     

液相色谱-串联质谱法测定牛乳基婴幼儿配方奶粉中的乳铁蛋白

目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定牛乳基婴幼儿配方奶粉中的乳铁蛋白含量的方法。方法试样中的乳铁蛋白经尿素-碳酸氢铵缓冲液提取,二硫苏糖醇还原,碘乙酰胺烷基化,37℃酶解后,特征肽段用液相色谱-串联质谱正离子模式测定,内标法定量。结果乳铁蛋白在0.00080-0.16 pmol/μL（相当于10~2000 mg/100 g）水平间线性关系良好,相关系数r≥0.9990,检出限为0.0020 pmol/μL,相当于25 mg/100g。检测结果加标回收率为92.00%~101.90%,相对标准偏差2.96%~4.15%。结论该方法准确好、特异性强、灵敏度高,可用于牛乳基婴幼儿配方奶粉中的乳铁蛋白含量的测定。     

婴幼儿配方奶粉中3-氯丙醇酯的GC-MS法测定及暴露危险分析

目的:建立婴幼儿配方奶粉中3-氯丙醇酯的气相色谱—质谱联用(GC-MS)测定方法,并对部分市售婴幼儿配方奶粉中3-氯丙醇酯的含量进行调查。方法:用乙醚+石油醚(1∶1)提取奶粉样品中脂肪,以1 m L甲醇钠甲醇溶液(0.25 mol/L)将脂肪中的3-氯丙醇酯(3-MCPD酯)水解成3-氯丙醇(3-MCPD)并用硅藻土小柱净化后,经七氟丁酰基咪唑衍生,再用选择离子监测的气相色谱—质谱联用法测定,采用内标法定量。结果:3-MCPD酯在250~5 000μg/kg范围内线性良好(r0.999),3个浓度水平下加标回收率为71.5%~99.6%,相对标准偏差为2.3%~6.0%。20份奶粉样品中,检出率65%,含量为0.26~0.97 mg/kg脂肪、0.042~0.22 mg/kg样品。不同阶段统计婴幼儿配方奶粉平均暴露量,一阶段3.32μg/(kg·bw)、二阶段2.42μg/(kg·bw)、三阶段2.72μg/(kg·bw)、四阶段0.23μg/(kg·bw)。结论:该方法灵敏度高、定量准确度,适合婴幼儿配方奶粉中3-氯丙醇酯的检测。     

婴幼儿配方奶粉中肌醇的测定及稳定性研究

建立了毛细管气相色谱-内标法测定婴幼儿配方奶粉中肌醇质量分数的方法。肌醇被体积分数为70%乙醇提取后,加入山梨醇为内标,经衍生试剂衍生,用正己烷萃取,采用氢火焰检测器(FID)的气相色谱仪检测。结果表明,肌醇的回收率是98.42%~100.97%,相对标准偏差(RSD)为0.54%~1.23%,线性范围在0~500μg之间,检出限为0.72 mg/100g。本方法可有效地减少基质中杂质的干扰,提高检测的准确性,与国标方法相比无显著性差异,适用于婴幼儿配方奶粉中肌醇质量分数的分析测定。同时采用本方法跟踪测定了婴幼儿配方奶粉开封后180 d内肌醇质量分数的变化情况,分析肌醇在婴幼儿配方奶粉中的稳定性。结果表明,肌醇质量分数随时间的延长而降低,在高温(37℃)存放时损失最快。     

ICP-OES法测定婴幼儿配方奶粉中钼的方法研究

建立电感耦合等离子体发射光谱法测定婴幼儿配方奶粉中的钼含量。此方法用微波消解法处理婴幼儿配方奶粉样品,然后运用电感耦合等离子体发射光谱法分析样品,同时探讨最佳消解奶粉样品和分析样品的条件。微波消解-电感耦合等离子体光谱法测定婴幼儿配方奶粉中的钼,方法在0~0.500 mg/L范围内线性关系良好(0.999 9),检出限可以达到0.048 mg/kg,6次奶粉样品测定结果的相对标准偏差小于3%;在加标量为0.2、1.0、2.0 mg/kg 3种梯度浓度下,回收率在96.6%~102%之间;标准参考物质的分析结果也在证书值范围内。该方法使用试剂少,空白值低,具有良好的精密度和准确度,适用于婴幼儿配方奶粉中钼的测定。     

HPLC法快速测定婴幼儿配方奶粉中维生素B_1

建立了快速测定婴幼儿配方奶粉中维生素B_1的高效液相色谱法。样品经水提取,饱和乙酸铅溶液沉淀蛋白,碱性铁氰化钾衍生,采用C_(18)色谱柱分离,以乙酸钠-甲醇(65∶35,V/V)为流动相,荧光检测器检测。该方法检出限为0.2 mg/kg,线性范围为0.01~1.0μg/m L,样品加标回收率在86.0%~88.8%之间。该方法样品前处理简便快速、测定结果符合定性定量要求,适用于婴幼儿配方奶粉中维生素B_1的测定。     

高效液相色谱法检测婴幼儿奶粉中的叶黄素

建立了一种使用高效液相色谱技术检测婴幼儿配方奶粉中游离、包埋叶黄素和叶黄素酯的方法。样品经室温皂化后用乙醚∶正己烷∶环己烷(40∶40∶20,体积比)组成的提取溶剂进行提取,以甲醇和甲基叔丁基醚为流动性,在C30色谱柱上采用梯度洗脱,可以很好的将13、13’-顺势叶黄素及反式叶黄素分离。对检测方法进行方法验证,在质量浓度为0.05~1.0 mg/L范围内其线性相关系数≥0.999,检出限为0.06μg/g,回收率在97.61%~108.6%之间,相对标准偏差为2.64%~4.54%。本方法操作简单、结果准确,适用于婴幼儿配方奶粉中游离、包埋叶黄素和叶黄素酯的测定。     

高效液相色谱-串联质谱法同时测定婴幼儿配方食品中香兰素、甲基香兰素和乙基香兰素

目的建立了高效液相色谱-串联质谱法同时测定婴幼儿食品中香兰素、甲基香兰素和乙基香兰素的方法。方法 样品经Tris溶液和乙腈振荡提取,离心后提取液用正己烷脱脂过滤后上机测定,外标法定量。结果 3种化合物在5.0~200μg/L范围内线性良好,在液态奶中测定低限均为25μg/kg,在奶粉中测定低限均为50μg/kg,方法加标收率在89.5%~115%之间,相对标准偏差(RSD)小于15.6%。结论 该方法简便、快速,准确,灵敏度及精密度高,适用于婴幼儿食品中香兰素、甲基香兰素和乙基香兰素的测定。     

山羊奶与牛奶和人奶营养成分的比较

对山羊奶、牛奶和人奶中蛋白质、脂肪、维生素、矿物质等主要营养成分进行了比较,分析了3种奶中主要营养成分的差别。通过比较发现,山羊奶在总体营养成分方面优于牛奶,更接近人奶。但山羊奶存在铁、叶酸和维生素B12含量较低以及羊奶膻味的问题,应在营养上对这方面加以重视。     

Calibration of infrared milk analyzers: modified milk versus producer milk

Mid-infrared (MIR) milk analyzers are traditionally calibrated using sets of preserved raw individual producer milk samples. The goal of this study was to determine if the use of sets of preserved pasteurized modified milks improved calibration performance of MIR milk analyzers compared with calibration sets of producer milks. The preserved pasteurized modified milk sets exhibited more consistent day-to-day and set-to-set calibration slope and intercept values for all components compared with the preserved raw producer milk calibration sets. Pasteurized modified milk calibration samples achieved smaller confidence interval (CI) around the regression line (i.e., calibration uncertainty). Use of modified milk calibration sets with a larger component range, more even distribution of component concentrations within the ranges, and the lower correlation of fat and protein concentrations than producer milk calibration sets produced a smaller 95% CI for the regression line due to the elimination of moderate and high leverage samples. The CI for the producer calibration sets were about 2 to 12 times greater than the CI for the modified milk calibration sets, depending on the component. Modified milk calibration samples have the potential to produce MIR milk analyzer calibrations that will perform better in validation checks than producer milk-based calibrations by reducing the mean difference and standard deviation of the difference between instrument values and reference chemistry.     

模拟母乳及婴儿配方奶粉的研究

介绍了人乳中的主要功能因子及其对婴儿的生长发育所具有的生理意义。比较、分析了现阶段婴儿配方奶粉与人乳成分中存在的差别及不足，并针对婴儿的生长特点及现阶段生产技术，对婴儿配方奶粉的生产及发展进行了叙述。     

Decreased milk yield is associated with delayed milk ejection

To determine whether individual cow milking vacuum (within the short milk tube and the liner mouthpiece) could be substituted for milk flow technology to identify delayed (bimodal) milk ejection, and the possible relationship between bimodal milk flow and milk yield, we recorded milking data from 663 Holstein cows on a 3,600-cow Michigan dairy that milked 3 times per day. Overall, delayed milk ejection occurred in 45.6% of the milkings, and 98% of the cows with delayed milk ejection also had bimodal flow. Multivariable analysis revealed that milk yield during each individual cow milking was positively associated with increasing lactation number but negatively associated with increasing days in milk and delayed milk ejection. As the time between unit attachment and the estimated milk letdown (the lag period) increased, milk yield decreased; relative to a lag of <30 s, milk yield decreased by 1.8 and 3.1 kg for lags of 30–59 and ≥60 s, respectively. The final multivariate model had an adjusted coefficient of determination of 0.27. The negative association between delayed milk ejection and decreased milk yield in this study suggested that milking vacuum parameters from individual cows could serve as a useful tool to qualitatively estimate milk flow within a herd and that this information may be used to enhance herd productivity.     

免疫学检测羊乳中掺入牛乳成分

由于营养、价格和原料等原因，市场上在羊乳中掺入牛乳的现象常有发生。针对这种乳源性掺假陆续产生了多种检测方法，本文主要综述了以ELISA为主的免疫学快速检测方法。     

Effects of milk powders in milk chocolate

The physical characteristics of milk powders used in chocolate can have significant impact on the processing conditions needed to make that chocolate and the physical and organoleptic properties of the finished product. Four milk powders with different particle characteristics (size, shape, density) and "free" milk fat levels (easily extracted with organic solvent) were evaluated for their effect on the processing conditions and characteristics of chocolates in which they were used. Many aspects of chocolate manufacture and storage (tempering conditions, melt rheology, hardness, bloom stability) were dependent on the level of free milk fat in the milk powder. However, particle characteristics of the milk powder also influenced the physical and sensory properties of the final products.     

Effect of leaving milk trucks empty and idle for 6 h between raw milk loads

The US Pasteurized Milk Ordinance (PMO) allows milk tanker trucks to be used repeatedly for 24 h before mandatory clean-in-place cleaning, but no specifications are given for the length of time a tanker can be empty between loads. We defined a worst-case hauling scenario as a hauling vessel left empty and dirty (idle) for extended periods between loads, especially in warm weather. Initial studies were conducted using 5-gallon milk cans (pilot-scale) as a proof-of-concept and to demonstrate that extended idle time intervals could contribute to compromised raw milk quality. Based on pilot-scale results, a commercial hauling study was conducted through partnership with a Pacific Northwest dairy co-op to verify that extended idle times of 6 h between loads have minimal influence on the microbiological populations and enzyme activity in subsequent loads of milk. Milk cans were used to haul raw milk (load 1), emptied, incubated at 30°C for 3, 6, 10, and 20 h, and refilled with commercially pasteurized whole milk (load 2) to measure cross-contamination. For the commercial-scale study, a single tanker was filled with milk from a farm known to have poorer quality milk (farm A, load 1), emptied, and refilled immediately (0 h) or after a delay (6 h) with milk from a farm known to have superior quality milk (farm B, load 2). In both experiments, milk samples were obtained from each farm's bulk tank and from the milk can or tanker before unloading. Each sample was microbiologically assessed for standard plate count (SPC), lactic acid bacteria (LAB), and coliform counts. Selected isolates were assessed for lipolytic and proteolytic activity using spirit blue agar and skim milk agar, respectively. The pilot-scale experiment effectively demonstrated that extended periods of idle (>3 h) of soiled hauling vessels can significantly affect the microbiological quality of raw milk in subsequent loads; however, extended idle times of 6 h or less would not measurably compromise milk quality in subsequent loads in commercial tankers. Current tanker sanitation practices appear to be sufficient for maintaining raw milk SPC, LAB, and coliform levels, which are important measures of milk quality.     

奶啤的研制

以牛奶、麦芽和酒花为主要原料,通过二次生物发酵研制出具有奶香和啤酒风味的奶啤饮料。通过实验确定奶啤的最佳配方及生产工艺流程并对奶啤的稳定性进行探讨,从而研制出即有啤酒的低酒精度、泡沫丰富和适度的二氧化碳,又具有酸乳饮料的酸甜可口、营养全面的奶啤饮料。     

Invited review: Corrected milk: Reconsideration of common equations and milk energy estimates

Corrected milk equations were developed in attempts to bring milk weights to a standardized basis for comparison by expressing the weight and composition of milk as corrected to the energy content of milk of a specific composition. Expressed as milk weights familiar on farm and in commerce, this approach integrates energy contributions of the dissimilar components to make the mass units more comparable. Such values are applied in evaluating feed efficiency, lactation performance, and global milk production, as functional units for lifecycle assessments, and in translation of research results. Corrected milk equations are derived from equations relating milk gross energy to milk composition. First, a milk energy equation is used to calculate the energy value of the milk composition to correct to (e.g., 0.695 Mcal/kg for milk with 3.5% fat, 3.05% true protein, and 4.85% lactose). That energy value is divided into the energy equation to give the corrected milk equation. Confusion has arisen, as different equations purport to correct to the same milk composition; their differences are based on uses of different energy equations or divisors. Accuracy of corrected milk equations depends on the accuracy of the energy equations used to create them. Energy equations have evolved over time as different milk component analyses have become more available. Inclusion of multiple milk components more accurately predicts milk energy content than does fat content alone. Omission of components from an equation requires the assumption that their content in milk is constant or highly correlated with an included component. Neither of these assumptions is true. Milk energy equations evaluated on a small data set of measured milk values have demonstrated that equations that incorporate protein, fat, and lactose contents multiplied by the gross energy of each component more closely predict milk energy than equations containing fewer components or regression-derived equations. This provides a tentative recommendation for using energy equations that include the 3 main milk components and their gross energy multipliers for predicting milk energy and deriving corrected milk equations. Accuracy of energy equations is affected by the accuracy of gross energy values of individual components and variability of milk composition. Lactose has consistent reported gross energy values. In contrast, gross energy of milk fat and protein vary as their compositional profiles change. Future refinements could assess accuracy of milk fat and protein gross energy and whether that appreciably improves milk energy predictions. Fat gross energy has potential to be calculated using the milk fatty acid profile, although the influence on gross energy may be small. For research, direct reporting of milk energy values, rather than corrected milk, provides the most explicit, least manipulated form of the data. However, provision of corrected milk values in addition to information on components can serve to translate the energy information to a form familiar to and widely used in the field. When reporting corrected milk data, the corrected milk equation, citation for the energy equation used, and composition and energy contents of the corrected milk must be described to make clear what the values represent.     

毛细管电泳法对乳及乳制品中乳源蛋白的研究

采用毛细管电泳方法对原料乳、市售鲜奶、不同厂家的巴氏灭菌乳、不同厂家和产地超高温灭菌乳(UHT)、调味乳、乳酸饮料、复原乳、酸奶、奶粉中蛋白成分进行检测。选择聚乙烯醇涂层毛细管,采用柠檬酸缓冲体系,在紫外检测214nm、分离电压20kV条件下对乳及乳制品中的α一乳白蛋白(α-La)、β一乳球蛋白(β-Lg)、α-酪蛋白(α-CN)、β-酪蛋白(β-CN)和k-酪蛋白(k-CN)进行分离测定。结果表明:五种蛋白的含量在原料乳(巴氏灭菌乳、市售鲜奶)、UHT乳、酸奶、调味乳、乳酸饮料、复原乳中依次降低,而UHT乳含量随保质期的增加而减少,奶粉中蛋白质含量因其适应人群而有差异。乳及乳制品中蛋白质的含量与其存在形式、产地及加工工艺相关。