快速检测复合预混合饲料中维生素D3含量的高效液相色谱法

建立了高效液相色谱测定复合预混合饲料中维生素D_3的分析方法。样品经水超声破解微粒包被,再用乙腈提取后,使用C_(18)色谱柱,采用紫外检测器,检测波长为264 nm,外标法定量。结果表明,维生素D_3在0.05～5μg/ml线性关系良好,相关系数(r)为0.999 9。方法定量限1.00×10~4 IU/kg,平均加标回收率82.1%～87.9%,相对标准偏差2.08%～3.20%。按上述方法共检测样品20批次,结果表明,该方法快速、准确可靠,能够实现快速测定预混合饲料中维生素D_3的含量。     

多波长快速测定巨鹿杏中有机酸和维生素含量及多地域杏产品比对研究

本文采用高效液相色谱-二极管阵列检测器法(HPLC-DAD)快速检测杏中水溶性有机酸(苹果酸,柠檬酸和琥珀酸)和维生素(维生素C、维生素B1、维生素B2)含量。以0.5 mmol/L磷酸-乙腈为流动相,随着时间推移改变流速和流动相比例,13 min内梯度洗脱,采用多检测波长210 nm,254 nm和270 nm条件下,可使所测有机酸和维生素实现快速较好地分离。方法的稳定性在0.75-2.12%范围内,精密度在0.94-1.55%之间,回收率测定结果为96.7-101.9%。采用本方法测定不同地域杏样品,提出巨鹿杏的特征性品质。     

高效液相色谱法测定米糠中的水溶性维生素

高效液相色谱法同时测定米糠中4种水溶性维生素VB1,VB6,烟酸,烟酰胺的含量。在HypersilC18(250cm×4.6mmid,5.0μm)上,以体积比为88∶12的0.1%磷酸水溶液-甲醇为流动相,以0.6mL/min流速等度洗脱,在266nm波长下检测。各组分在8min能基线分离。4种维生素在6×10-7～8.5×10-5g/mL范围内呈线性关系,VB1、VB6、烟酸和烟酰胺的检出下限分别为4.3×10-7、3.4×10-7、3.2×10-7、3.0×10-7mg/L。经简单预处理,可以对米糠和淘米水中的这4种维生素的含量进行测定,平均回收率在96.0%～99.9%之间。该法简便、快速、准确、灵敏,对复杂体系水溶性维生素的测定具有重要的参考价值。     

液质联用仪同步检测婴幼儿配方食品中11种水溶性维生素

建立高效液相色谱-串联质谱测定婴幼儿配方食品中11种水溶性维生素的同步检测方法。样品经过前处理后,采用Waters ACOUTITY UPLC HSS T3(2.1×100 mm,1.8μm)色谱柱进行分离;流动相为0.1%甲酸的甲醇溶液和10 mmol/L甲酸铵水溶液(p H=3.5),梯度洗脱,采用电喷雾离子源多反应监测(MRM)模式进行检测。结果表明,11种水溶性维生素在5 min内完成一个样品的分析,线性关系良好(r≥0.999),方法检出限在0.02~3.00 ng/m L之间。在三个水平添加回收率试验,每个水平重复5次,其平均回收率在88.0%~110.0%之间,测定结果的相对标准偏差小于5%。该方法具有快速、简单、准确、灵敏等特点,可对较宽浓度范围内的多种维生素进行同步分析,有助于提高食品检测实验室的分析效率,降低成本。可用于婴幼儿配方食品中水溶性维生素的检测。     

HPLC法测定保健食品B族维生素片中9种维生素B的含量

目的:建立高效液相色谱-二极管阵列检测（HPLC-DAD）法测定B族维生素片中9种维生素B成分的含量。方法:样品中的叶酸经0.3%氨溶液超声提取,样品中的生物素、维生素B₁₂和泛酸经水超声提取,样品中的维生素B₁、维生素B₂、维生素B₆、烟酸和烟酰胺经0.1%盐酸超声提取,经C₁₈柱分离,以甲醇-0.1 mol/L磷酸二氢钾溶液为流动相进行梯度洗脱,泛酸和生物素在205 nm波长处进行检测,维生素B₁、维生素B₂、烟酸和烟酰胺在256 nm波长处进行检测,维生素B₆和叶酸在287 nm波长处进行检测,维生素B₁₂在361 nm波长处进行检测。结果:9种成分能实现较好地分离,在各自线性范围内线性关系良好,决定系数R2均大于0.999,平均回收率为91.8%~106.9%,RSD为0.2%~4.8%,方法的检出限在0.05~4.7 mg/kg之间。结论:该方法操作快速简便、精密度和重复性好,能快速完成保健食品B族维生素片中9种维生素B成分的测定,并降低成本。     

高效液相色谱-串联质谱法测定保健食品中 10种水溶性维生素

目的建立高效液相色谱-串联质谱法检测保健食品中10种水溶性维生素的分析方法。方法采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS),ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以0.1%甲酸水溶液为流动相A,0.1%甲酸的甲醇溶液为流动相B,梯度洗脱。通过分子离子峰、二级碎片、色谱保留时间等信息,对保健食品中10种水溶性维生素进行鉴别和定量测定。结果 10种水溶性维生素实现了同时分离与专属鉴定,维生素B_1在0.01~1μg/mL的浓度范围内线性关系良好(r0.995);维生素C在0.1~50μg/mL的浓度范围内线性关系良好(r0.995);其他8种维生素在0.01~10μg/mL的浓度范围内线性关系良好(r0.995),高、中、低不同浓度的加标回收率在80%~120%之间,精密度在0.3%~3%之间。结论本方法专属性强、灵敏度高,结果准确可靠,可以作为片剂和口服液基质保健食品中检测水溶性维生素的方法参考。     

超高效液相色谱-同位素稀释质谱法同时测定婴幼儿配方奶粉中10种水溶性维生素

目的建立超高效液相色谱-同位素稀释质谱法(ultra performance liquid chromatography-isotope dilution mass spectrometry, UPLC-IDMS)同时检测婴幼儿配方奶粉中10种水溶性维生素(维生素B1、维生素B2、烟酸、烟酰胺、吡哆醇、吡哆醛、吡哆胺、泛酸、生物素、叶酸)的方法。方法样品用水溶解后,加入同位素内标,用1 mol/L盐酸溶液调节pH至1.7,再用1 mol/L NaOH溶液调节pH至4.5,经Agilent ZORBAX SB-AQ C18色谱柱(100 mm×3.0 mm, 1.8μm)分离,正离子模式下以0.2%甲酸水溶液和甲醇-乙腈(4:6,V:V)为流动相,负离子模式下以水和甲醇-乙腈(4:6,V:V)为流动相梯度洗脱,采用电喷雾离子源,分别在正、负离子模式下进行多反应监测模式测定,内标法定量。结果 10种水溶性维生素在10～5000ng/mL内具有良好的线性关系,相关系数(r~2)大于0.99,加标回收率为85.7%～115.8%,相对标准偏差为1.82%～9.67%。结论该方法简便、快速、灵敏、准确,可满足婴幼儿配方奶粉中水溶性维生素的检测要求。     

高效液相色谱法检测婴幼儿配方食品中维生素B12的含量

目的 建立一种高效液相色谱快速检测婴幼儿配方食品中维生素B12的方法。方法 选择C18柱（250×4.6mm,4.6 μm）作为色谱柱,流动相为水-甲醇（75:25）,流速0.5 mL/min等度洗脱,进样量35 μL,柱温40℃,波长361nm,样品经超声提取15 min,然后在8000 r/min下冷冻离心10 min,离心结束后取上清液过0.22 μm滤膜,上机测试。结果 显示维生素B12标准品在浓度0.05~2.0 μg/mL范围内线性良好;相关系数r=0.9998;平均回收率91.3 %;检出限2 ng/mL。结论 该条件下的高效液相色谱可测定婴幼儿配方食品中维生素B12含量,具有重复性好、简单、快速、结果准确等优点。因此该方法可应用于婴幼儿配方食品中维生素B12含量的检测。     

亲水高效液相色谱法测定饮料中的维生素C含量

目的:建立一种简便、快速、灵敏的测定饮料中维生素C含量的方法。方法:采用氨基丙基色谱柱Agilent Zorbax carbohydrate(250mm×4.6mm,5μm),流动相为0.02mol/L磷酸二氢钾+甲醇=95+5,流速1.0m L/min,检测波长:249nm,柱温:25℃,测定饮料中的维生素C含量。该方法检测线性范围为1.46~146μg/m L,样品检出限为0.08μg/m L,加样回收率为99.34%。结论:该方法利用亲水色谱的原理,使用氨基丙基色谱柱分析饮料中维生素C的含量,克服了传统液相色谱方法维生素C在C18柱上保留不足的问题,能够实现样品中杂质与目标峰的有效分离,且前处理简单,测定准确、简便、快速,是一种更为实用快速的维生素C的液相色谱分析方法。     

高效液相色谱法测定保健食品中维生素D3的含量

目的建立用半制备型反相高效液相色谱系统纯化、正相高效液相色谱硅胶柱色谱分离测定保健食品中维生素D_3含量的方法。方法通过皂化排除样品中的干扰物质,再经乙醚萃取浓缩,将浓缩后供试品溶液注入反相高效液相色谱仪净化分离去除杂质,排除维生素A的干扰,再用正相分析色谱进行定量分析,以正己烷-正戊醇(997:3,V:V)为流动相,流速为1.0 mL/min,采用色谱柱Waters Nova-Pak?Silia分离,在254 nm检测波长下经紫外或二极管阵列检测器检测,外标法定量。结果维生素D_3浓度在0.297~9.506μg/mL范围内呈良好的线性关系,相关系数为1,平均回收率为100.55%~100.58%,相对标准偏差值为0.44%~0.72%。结论该方法快速准确,可适用于保健食品中维生素D_3含量的测定。     

高效液相色谱法快速测定多维片中的维生素B12

目的建立高效液相色谱法快速测定多种维生素片中的维牛素B_(12)含量。方法样品用水作为溶剂经超声波提取,以0.02 mol/L磷酸二氢钾溶液(pH=2.5)和乙腈作为流动相采用高效液相色谱法测定,以外标法定量。结果本研究将检测波长改为546 nm,可减少多维片中其他组分的干扰。维生素B_(12)在0.5~10 mg/L范围内线性关系良好(r=0.9999),在1、2和5 mg/L的添加水平下测得回收率分别为98.1%、97.2%和99.0%(n=6),相对标准偏差分别为3.6%、2.0%和4.6%,方法检出限为0.2 mg/L,定量限为0.5 mg/L。结论该方法快速、简便、准确且干扰少,可适合于多种维生素片中维生素B_(12)的定量分析。     

反相高效液相色谱法测定果醋中的8 种维生素

建立梯度洗脱反相高效液相色谱法同时检测果醋中VC、VB1、VB2、VB3、VB6、VB12、叶酸和烟酰胺8种水溶性维生素的分析方法。考察柱温、缓冲液浓度、pH值以及梯度洗脱程序对各组分分离的影响。最终采用0.1mol/L醋酸钠溶液(pH4.25)和甲醇作为流动相进行梯度洗脱,流速为1.00mL/min,柱温为30℃,8种水溶性维生素在14.2min内达到基线分离;紫外检测波长为266nm和280nm;线性范围：VB2、叶酸为0.05～12.5μg/mL;VC、VB1、VB3、烟酰胺为0.1～25μg/mL;VB6、VB12为0.15～37.5μg/mL,相关系数均在0.999以上,其最低检出限为0.47～3.46ng/mL。该法被成功地用于定量果醋中的维生素,平均加标回收率为92.4%～105.2%,相对标准偏差为0.08%～1.54%。     

Development of an Analytical Method for the Combined Determination of Water-Soluble Vitamins and Minerals Through High-Performance Liquid Chromatography–Inductively Coupled Plasma Atomic Emission Spectrometry Hyphenation

The capabilities of inductively coupled plasma atomic emission spectrometry (ICP-AES) for the determination of water-soluble vitamins after high-performance liquid chromatography (HPLC) separation have been evaluated for the first time in the present work. Thanks to the multielemental capability of ICP-AES, it has been possible to develop a method for the joint determination of several water-soluble vitamins and minerals. The vitamin chromatograms were obtained by plotting the carbon corrected emission intensity against time. Meanwhile, minerals were determined through the measurement of the emission intensity at their characteristic wavelengths. The established method was applied to the determination of thiamine, riboflavin, pantothenic acid, nicotinamide, ascorbic acid, Cr, Mo, Se, Mn, Zn, Fe, Mg, Ca, and K in multivitamin complexes. Good linearities were obtained, with correlation coefficients above 0.999 for all the vitamins and metals. The detection limits using ICP-AES for vitamins were lower than 10 mg L⁻¹ except for biotin (18 mg L⁻¹) and ascorbic acid (35 mg L⁻¹). Moreover, the limits of detection for metals ranged from 0.3 mg L⁻¹ for K and 0.02 mg L⁻¹ for Mo. Even though the ICP is less sensitive than PDA and MS for vitamin determination, the HPLC-ICP-AES allows determination of vitamins and minerals in a period of time not much higher than that required for the simple determination of the minerals, and it is less sensitive to interferences in trace quantities.     

钛胶RP-HPLC法同时测定5 种维生素

采用钛胶反相色谱柱,建立高效液相色谱法同时测定5 种维生素：烟酸、生物素、烟酰胺、叶酸和钴胺素含量的检测方法。研究5 种维生素的保留行为与磷酸缓冲盐pH值、缓冲盐类型及浓度、柱温和流速的关系,得出了最优色谱条件：于波长210 nm处检测生物素和钴胺素,于波长270 nm处检测烟酸、烟酰胺和叶酸,磷酸盐pH 7.0,浓度5.0 mmol/L,柱温50 ℃,流速0.8 mL/min。分析5 种维生素保留的热力学参数焓、熵和吉布斯自由能。烟酸、生物素、烟酰胺、叶酸和钴胺素标准曲线线性良好（R2＞0.999 0）;烟酸、生物素、烟酰胺、叶酸和钴胺素的检出限分别为6、10、20、22、8 ng/mL;5 种物质的相对标准偏差均低于1.36%;加标回收率范围为92.30%～107.20%。方法的精密度和准确度均可满足高效液相色谱法的测定要求。     

强化淀粉类食品中7 种水溶性维生素的快速测定

建立高效液相色谱-二极管阵列-荧光联用法同时检测营养强化淀粉类食品中7 种水溶性维生素含量的方法。样品经淀粉酶60 ℃酶解45 min,调pH值提取后,经十二烷基硫酸钠（5 mmol/L,加入0.1%磷酸,三乙胺调pH 3.0）-乙腈梯度洗脱,VB1、烟酸、烟酰胺在不同波长下进行检测,VB2、吡哆醛、吡哆醇、吡哆胺采用目标物出峰时间段转变激发、发射波长检测。7 种维生素在各自线性范围内线性关系良好,相关系数r2为0.999 6～0.999 9,加标回收率为90.5%～102.5%,检出限为0.01～0.08 mg/100 g,定量限为0.025～0.26 mg/100 g。方法快速、高效,适用于大批量强化淀粉类食品中7 种水溶性维生素的同时测定。     

Determination of water-soluble vitamins using a colorimetric microbial viability assay based on the reduction of water-soluble tetrazolium salts

A method for the determination of water-soluble vitamins using a colorimetric microbial viability assay based on the reduction of the tetrazolium salt {2-(2-methoxy-4-nitrophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfophenyl)-2H-tetrazolium, monosodium salt (WST-8)} via 2-methyl-1,4-napthoquinone (NQ) was developed. Measurement conditions were optimized for the microbiological determination of water-soluble vitamins, such as vitamin B₆, biotin, folic acid, niacin, and pantothenic acid, using microorganisms that have a water-soluble vitamin requirement. A linear relationship between absorbance and water-soluble vitamin concentration was obtained. The proposed method was applied to determine the concentration of vitamin B₆ in various foodstuffs. There was good agreement between vitamin B₆ concentrations determined after 24 h using the WST-8 colorimetric method and those obtained after 48 h using a conventional method. The results suggest that the WST-8 colorimetric assay is a useful method for the rapid determination of water-soluble vitamins in a 96-well microtiter plate.     

RP-HPLC 法测定功能性饮料水溶性维生素含量

目的：建立同时测定功能性饮料中VC、VPP、VB6、VB2 和VB1 水溶性维生素含量的RP-HPLC 方法。方法：色谱条件：色谱柱：Luna C18(2)(200mm ×4.60mm,5μm),流动相：0.005mol/L 己烷磺酸钠溶液- 甲醇-冰醋酸(80:20:0.5,V/V)(pH4.0),流速1.0mL/min,检测波长278nm。结果：VC、VPP、VB6、VB2 和VB1 的线形范围分别是2.94～43.50、6.00～90.00、1.70～25.50、1.60～24.00、2.30～43.50μg/mL,最低检出限分别为0.001、0.362、0.095、0.328、0.619μg/mL;VC、VPP、VB6 平均回收率分别为98.29%、98.38%、98.51%。结论：此方法简单、快捷、准确,可同时测定功能性饮料中的多种水溶性维生素。     

Simultaneous determination of water-soluble vitamins in beverages and dietary supplements by LC-MS/MS

An LC-MS/MS method was developed for the simultaneous determination of 15 water-soluble vitamins that are widely used as additives in beverages and dietary supplements. This combined method involves the following simple pre-treatment procedures: dietary supplement samples were prepared by centrifugation and filtration after an extraction step, whereas beverage samples were diluted prior to injection. Chromatographic analysis in this method utilised a multi-mode ODS column, which provided reverse-phase, anion- and cation-exchange capacities, and therefore improved the retention of highly polar analytes such as water-soluble vitamins. Additionally, the multi-mode ODS column did not require adding ion pair reagents to the mobile phase. We optimised the chromatographic separation of 15 water-soluble vitamins by adjusting the mobile phase pH and the organic solvent. We also conducted an analysis of a NIST Standard Reference Material (SRM 3280 Multi-vitamin/Multi-element tablets) using this method to verify its accuracy. In addition, the method was applied to identify the vitamins in commercial beverages and dietary supplements. By comparing results with the label values and results obtained by official methods, it was concluded that the method could be used for quality control and to compose nutrition labels for vitamin-enriched products.     

Inhibition of acrylamide formation by vitamins in model reactions and fried potato strips

The capacities of 15 vitamins in reducing the formation of acrylamide were examined. Inhibitory activities of the water-soluble vitamins were tested in both chemical models containing acrylamide precursors (asparagines and glucose) and a food model system (fried snack products), while activities of fat-soluble vitamins were examined only in the latter model. Biotin, pyridoxine, pyridoxamine, and l-ascorbic acid exerted a potent inhibitory effect (>50%) on acrylamide formation in the chemical model system. Using the food model, it was shown that water-soluble vitamins are good inhibitors of acrylamide formation. On the other hand, only weak inhibitory effects were observed with fat-soluble vitamins. Effects of pyridoxal, nicotinic acid, and l-ascorbic acid were further examined using fried potato strips. Nicotinic acid and pyridoxal inhibited acrylamide formation in fried potato strips by 51% and 34%, respectively. Thus, certain vitamins at reasonable concentrations can inhibit the formation of acrylamide.