高效液相色谱法同时测定食品中的12种抗氧化剂

目的：建立一种快速、准确测定食品中12 种抗氧化剂的高效液相色谱法。方法：样品用正己烷溶解,用含抗坏血酸棕榈酸盐(AP)的饱和乙腈萃取,以反相C18 柱为分离柱,以甲醇- 乙腈- 乙酸- 水体系为流动相进行梯度洗脱,采用高效液相色谱- 紫外检测器于280nm 定量检测。结果：12 种抗氧化剂在36min 内完全分离,线性范围为0.2～200mg/L(r=0.9981～0.9999),定量限为0.2～1.0mg/kg,回收率为81.13%～107.57%,相对标准偏差为0.26%～4.52%(n=7)。结论：本方法准确、可靠、简便、检出限低,适合分析大批量样品。     

化妆品中柠檬酸检测能力验证结果分析

目的考察相关实验室检测化妆品中柠檬酸的技术能力和水平,促进参加实验室对该类项目检验能力的提高。方法样品通过均匀性和稳定性评价后,采用随机单盲方式分配至参与能力验证(proficiency testing,PT)的实验室。统计各参加实验室的测定结果,进行稳健统计分析,通过Z比分数评价实验室检测能力。结果制备的200瓶样品均匀性符合要求且在整个计划周期内保持稳定,满足能力验证计划要求。从参加的31家的结果来看,共有27家满意,满意率为87.1%。结论化妆品中柠檬酸的检测水平总体良好,个别实验室检测能力有待提高。     

高效液相色谱法同时测定食品接触材料水性模拟物中三聚氰胺和苯代三聚氰胺

建立了食品接触材料水性模拟物中三聚氰胺和苯代三聚氰胺的高效液相色谱（HPLC）分析方法。样品根据拟装食品类型不同,经水、3%（w/v）乙酸水溶液、4%（v/v）乙酸水溶液、10%（v/v）乙醇水溶液、20%（v/v）乙醇水溶液或50%（v/v）乙醇水溶液6种不同水性模拟物提取,0.45μm滤膜过滤后直接由高效液相色谱分析。色谱分离采用强阳离子交换与反相C18混合填料分析柱（混合比例1∶4）,柱温35℃,流动相为乙腈-20mmol/L乙酸铵缓冲溶液（pH3.0）（40∶60,v/v）,流速为0.2mL/min,检测波长为240nm。结果表明:在优化的条件下,三聚氰胺和苯代三聚氰胺标准品在0.2²0mg/L浓度范围内,线性相关系数为0.9997⁰.9999,方法定量限（S/N>10）为0.015⁰.033mg/dm2。在0.025⁰.70mg/dm2三个水平加标测试,平均回收率在80.0%¹03.3%之间,相对标准偏差（n=6）为0.5%⁴.0%。该方法前处理简单、分析速度快,可用于食品接触材料水性模拟物中三聚氰胺和苯代三聚氰胺的同时检测。      

超高效液相色谱法同时测定酱腌菜中的7种防腐剂与2种甜味剂

目的 建立采用超高效液相色谱(UPLC)-二极管阵列检测器(PDA)同时快速检测酱腌菜中7种防腐剂(山梨酸、苯甲酸、脱氢乙酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)和2种甜味剂(糖精钠、安赛蜜)的方法.方法 采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为甲醇+ 0.02 mol/L乙酸铵溶液,梯度洗脱,在35℃柱温,0.20 ml/min流速下,采用二极管阵列检测器在230、257 nm波长处进行检测,外标法定量.结果 2种甜味剂和7种防腐剂15 min内完全分离,在10～250 mg/L范围内,峰面积和质量浓度的线性关系良好(r≥0.999 1),以3组高、中、低浓度作为不同的添加水平,平均加标回收率为85.1％ ～98.8％,RSD为3.5％～8.5％(n=6),检出限(S/N=3)为0.2～ 1.0 mg/kg,定量限(S/N=10)为0.5～4.0 mg/kg.结论 本方法操作方便、分离效果好、线性范围宽,能满足酱腌菜中防腐剂和甜味剂的检测要求.     

利用高效液相色谱验证回锅油的品质

回锅油从外观上很难辨别好坏,甚至测定的酸价均在国标范围内,只能从内在的本质如脂肪酸的组成上验证。利用高效液相色谱(HPLC)测定回锅油中的脂肪酸成分,结果发现食用油在煎炸的前2h营养价值急剧下降(从85%降到17%),增加的游离脂肪酸却很少(从6mgKOH/g增加到14mgKOH/g),与前期测定的酸价的实验结果相符。说明可以用高效液相色谱来验证回锅油的品质,鉴别食用油的好坏。     

Agaritine content of 53 Agaricus species collected from nature

Fifty-three different species of the genus Agaricus were collected in the Czech Republic during the period 1998–2001 and identified by an experienced mycologist. The samples were analysed for agaritine (N ²-(γ-L-glutamyl)-4-hydroxymethylphenylhydrazine) content, a precursor to a suspected rodent carcinogen. There was a huge variation in agaritine content between species, but less variation between samples of a species. Whereas the cultivated mushroom Agaricus bisporus commonly contain 200–500 mg agaritine kg^?1 fresh weight, no less than 24 of the 53 species contained agaritine levels above 1000 mg kg^?1 fresh weight. The highest level was found in A. elvensis containing up to 10, 000 mg kg^?1 fresh weight. Twenty species contained intermediate levels (100–1000 mg kg^?1), and nine species were below 100 mg kg^?1. Some of the species producing low levels of agaritine might be candidates for future strain development of Agaricus mushrooms for cultivation. No correlation could be observed between agaritine content and size of the mushroom, week of the year when collected, year of collection, or site of collection. Besides occurring in the genus Agaricus, some species of the genera Leucoagaricus and Macrolepiota were also shown to contain agaritine.     

Formation of fumonisins and other secondary metabolites by Fusarium oxysporum and F. proliferatum: a comparative study

The principal aim of this study was to estimate the formation of fumonisins (FB₁ and FB₂), moniliformin (MON), and ergosterol (ERG) by Fusarium oxysporum and Fusarium proliferatum, while the formation of beauvericin (BEA) was estimated by the latter Fusarium species only. Moreover, the effect of temperature on the biosynthesis of mycotoxins was also evaluated. Fumonisins were formed by F. proliferatum, with the highest yield at 18°C (720.0–1976.6 µg g^?1 for FB₁, 74.2–670.8 µg g^?1 for FB₂) and only by three of four F. oxysporum strains at a very low level (0.02–4.77 µg g^?1 for FB₁, 0.02–2.15 µg g^?1 for FB₂). The amount of MON formed by F. proliferatum was the highest (p < 0.001) at 32°C (3056.87 µg g^?1), while MON biosynthesis by F. oxysporum was lower 227.54 µg g^?1 (p < 0.001). BEA was produced by F. proliferatum with the highest level at 25°C (p < 0.001). ERG–recognized as an indicator of fungal biomass development and as a consequence of mycotoxin formation–was found at the highest concentration at a biosynthesis temperature of 25°C for F. proliferatum and F. oxysporum (p < 0.001).     

Survey of aflatoxins in retail samples of whole and ground black and white peppercorns

A total of 126 local and imported samples of commercial white and black pepper in Malaysia were analysed for aflatoxins B₁, B₂, G₁ and G₂ (AFB1, AFB2, AFG1, AFG2) content using high-performance liquid chromatography (HPLC) with a fluorescence detector (FD). An acetonitrile–methanol–water (17 : 29 : 54; v/v) mixture was used as a mobile phase and clean-up was using an immunoaffinity column (IAC). Seventy out of 126 (55.5%) samples were contaminated with total aflatoxins, although only low levels of aflatoxins were found ranging from 0.1 to 4.9 ng g^?1. Aflatoxin B₁ showed the highest incidence of contamination and was found in all contaminated samples. There was a significant difference between type of samples and different brands (p < 0.05). The results showed black peppers were more contaminated than white peppers.     

高效液相色谱法测定牛奶中林可霉素的残留量

研究建立牛奶中林可霉素残留量的高效液相色谱测定方法。样品用水相提取,离心分离,经C18固相萃取柱净化,在210nm波长下用二极管矩阵检测器检测。色谱柱为Agilent ZORBOX SBC18柱(4.6×250mm,5μm),以0.05mol/L硼砂溶液(用磷酸调节pH6.0)-甲醇(55:45,V/V)为流动相,流速1.0ml/min。林可霉素浓度在1.0～10.0μg/g范围内与峰面积呈良好的线性关系,平均回收率为82.9%～93.1%,变异系数为1.45%～4.58%,最低检测限为0.5μg/ml。本方法简便、快速、准确。     

高效液相色谱法测定丽石黄衣中松萝酸的含量及抑菌活性的研究

以丽石黄衣(Xan thoria elegans (Link)Th.Fr.)为材料,乙酸乙酯为溶剂回流提取松萝酸,采用高效液相色谱法测定松萝酸的含量并用滤纸片法对松萝酸的抑菌作用进行了测定。实验结果表明,丽石黄衣中松萝酸的总含量为4.06%,松萝酸对酵母没有抑菌作用,可对其他受试细菌和真菌有抑菌作用。     

芹菜提取物中芹菜素的HPLC与HPTLC定量分析研究

通过采用高效液相色谱(HPLC)、紫外光谱和黄酮颜色特征反应对芹菜提取物主要成分芹菜素进行定性鉴定,同时建立定量测量芹菜素的高效薄层色谱(HPTLC)方法.结果表明:芹菜提取物的主要成分是黄酮醇.芹菜素,与芹菜素标准品具有相同的光谱和色谱性质;采用G60高效硅胶板,以氯仿-甲醇-水(18:2.3:0.35)为展开剂,芹菜素标样与试样有相同的Rf值为0.65;用最小二乘法作线性回归,芹菜素含量与斑点峰面积的标准曲线回归方程:y=15138x 7594.8,R2=0.993,线性范围:0.332～0.996μg/斑点.精密度实验RSD(n=5)=1.33%,平均回收率97.82%.     

Comparison of extraction solvents and conditions for herbicide residues in milled rice with liquid chromatography-diode array detection analysis (LC-DAD)

Different extraction procedures and clean-up methods were compared in order to develop a sample preparation procedure for the multi-residue analysis of six post-emergence herbicides (metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium and cyhalofop butyl) in rice grains followed by liquid chromatography-diode array detection (LC-DAD). Optimum results were obtained dispersing milled rice grain in water, followed by the addition of 1% acetic acid in acetonitrile, MgSO₄ and sodium acetate as a modification of the quick, easy, cheap, effective, rugged and safe (QuEChERS) method but no primary and secondary amine (PSA) sorbent was added due to the acidic nature of the herbicides. The method was further expanded to other post-emergence herbicides (quinclorac, clomazone and propanil). Except for quinclorac, which cannot be analysed with this method, the recoveries of the other eight herbicides were in the range 73–111%, with relative standard deviations lower than 12%. Limits of detection (LODs) ranged from 0.03 to 0.08 mg kg^?1. A single analyst can extract twelve samples in 4 h. The method presented here allows the simultaneous residue determination of the most common post-emergence herbicides employed in cultivating rice. It is simple, rapid, sensitive, and can be applied routinely to polished rice grain herbicide residue analysis.     

高效液相色谱柱前衍生法测定蜜饯中的甜蜜素

目的：建立简便、准确、灵敏的测定蜜饯中甜蜜素含量方法。方法：在酸性介质条件下,溶液中的甜蜜素同次氯酸钠溶液发生反应,其衍生产物在紫外-HPLC 法下测定。结果：方法最低检出限为0.05g/kg,其在0.02～1.00mg/ml 范围内呈线性关系,相关系数为0.9995,方法的相对标准偏差为1.56%～4.49%,回收率为91.5%～98.5%,检测结果与GB/T5009.97 - 2003 气相色谱法无显著差异。结论：本法灵敏度高,操作简单,稳定性和重复性好,适合于蜜饯中甜蜜素含量的测定。     

不同红茶中主要氨基酸含量及其对小鼠自主活动的影响研究

通过高效液相色谱法（HPLC）测定不同红茶中γ-氨基丁酸（γ-aminobutyric acid,GABA）、L-茶氨酸和L-谷氨酸的含量,并通过小鼠自主活动测试仪比较不同主要氨基酸含量的红茶水提物对小鼠自主活动的影响。结果表明,不同红茶中GABA、L-茶氨酸和L-谷氨酸含量差别均较大,并且L-茶氨酸含量普遍高于GABA、L-谷氨酸含量。其中,GABA含量以高黎贡山为最高,汉水韵红茶次之,紫鹃红最低;L-茶氨酸和L-谷氨酸含量均以八仙红茶为最高,汉水韵红茶次之,印度大吉岭红茶最低。此外,动物实验结果显示,与主要氨基酸含量较低红茶组相比,主要氨基酸含量较高红茶组小鼠的自主活动次数显著减少（p<0.05）。以上结果提示,主要氨基酸含量较高的红茶对小鼠具有明显的镇静作用。      

Monitoring of free glutamic acid in Malaysian processed foods,dishes and condiments

A study to quantify the free glutamic acid content of six processed foods, 44 dishes and 26 condiments available in Malaysia was performed using high-performance liquid chromatography with a fluorescence detector (HPLC-FRD). Recovery tests were carried out with spiked samples at levels from 6 to 31 mg g^?1. High recovery in different matrices was achieved ranging from 88% ± 13% to 102% ± 5.12%, with an average of 97% ± 8.92%. Results from the study revealed that the average free glutamic acid content ranged from 0.34 ± 0.20 to 4.63 ± 0.41 mg g^?1 in processed foods, while in prepared dishes it was as low as 0.24 ± 0.15 mg g^?1 in roti canai (puffed bread served with curry or dhal) to 8.16 ± 1.99 mg g^?1 in dim sum (a small casing of dough, usually filled with minced meat, seafood, and vegetables, either steamed or fried). Relatively, the content of free glutamic acid was found to be higher in condiments at 0.28 ± 0 mg g^?1 in mayonnaise to 170.90 ± 6.40 mg g^?1 in chicken stock powder.     

高效液相色谱法测定保健食品多维康胶囊中叶酸的含量

目的 建立高效液相色谱法(high performance liquid chromatography,HPLC)测定多维康胶囊中叶酸含量的方法.方法 采用C18(150 mm×4.6 mm,5μm)色谱柱,以磷酸二氢钾-甲醇溶液为流动相,流速0.8 mL/min,检测波长254 nm,柱温30℃,进样体积10μL.结...     

Carotenoid composition and vitamin A value in ají (Capsicum baccatum L.) and rocoto (C. pubescens R. & P.), 2 pepper species from the Andean region

The carotenoid patterns of fully ripe fruits from 12 Bolivian accessions of the Andean peppers Capsicum baccatum (ají) and C. pubescens (rocoto) were determined by high-performance liquid chromatography (HPLC)-photodiode array detector (PDA)-mass spectrometry (MS). We include 2 California Wonder cultivars as C. annuum controls. A total of 16 carotenoids were identified and differences among species were mostly found at the quantitative level. Among red-fruited genotypes, capsanthin was the main carotenoid in the 3 species (25% to 50% contribution to carotenoid fraction), although ajíes contained the lowest contribution of this carotenoid. In addition, the contribution of capsanthin 5,6-epoxide to total carotenoids in this species was high (11% to 27%) in comparison to rocotos and red C. annuum. Antheraxanthin and violaxanthin were, in general, the next most relevant carotenoids in the red Andean peppers (6.1% to 10.6%). Violaxanthin was the major carotenoid in yellow-/orange-fruited genotypes of the 3 species (37% to 68% total carotenoids), although yellow rocotos were characterized by lower levels (<45%). Cis-violaxanthin, antheraxanthin, and lutein were the next most relevant carotenoids in the yellow/orange Andean peppers (5% to 14%). As a whole, rocotos showed the highest contributions of provitamin A carotenoids to the carotenoid fraction. In terms of nutritional contribution, both ajíes and rocotos provide a remarkable provitamin A activity, with several accessions showing a content in retinol equivalents higher than California Wonder controls. Furthermore, levels of lutein in yellow/orange ajíes and rocotos were clearly higher than California Wonder pepper (≥1000 μg·100/g). Finally, the Andean peppers, particularly red ajíes, can be also considered as a noticeable source of capsanthin, the most powerful antioxidant compound among pepper carotenoids. Practical Application: Capsicum peppers are known for their content in carotenoids, although there is no information about 2 species with Andean origin: ajíes and rocotos. Due to their relevance for the Andean cuisine and increasing importance in ethnic restaurants in Europe, we studied their carotenoid pattern and vitamin A contribution.     

Occurrence of ochratoxin A and citrinin in Czech cereals and comparison of two HPLC methods for ochratoxin A detection

The aims of the study were to obtain information about the occurrence of ochratoxin A (OTA) and citrinin (CIT) in cereals harvested in the Czech Republic and to compare two analytical procedures for detecting OTA. A total of 34 cereal samples, including two matrix reference materials (R-Biopharm, Germany), were analysed. The results were compared with the limit for raw cereal grains used as a foodstuff according to Commission Regulation No. 1881/2006, which allows a maximum OTA level of 5 µg kg^?1. Compared were two methods based on the high-performance liquid chromatography principle, one using the immunoaffinity columns OchraTest? (VICAM) and the second based on solvent partition (PART), both followed by fluorescence detection. The highest OTA contents were found in two barley samples. According to the method employed, the results for the first sample (malting barley) were VICAM = 31.43 µg kg^?1 and PART = 44.74 µg kg^?1. For the second sample (feeding barley) they were VICAM = 48.63 µg kg^?1 and PART = 34.40 µg kg^?1. Two samples of bread wheat had an OTA content approaching the legal limit (VICAM = 4.71 µg kg^?1 and PART = 6.03 µg kg^?1; VICAM = 4.12 µg kg^?1 and PART = 3.95 µg kg^?1). CIT was analysed using the PART method only, and its highest content (93.64 µg kg^?1) was found for the malting barley sample with high OTA content (44.74 µg kg^?1 as analysed using PART).