Influence of putrescine,cadaverine, spermidine or spermine on the formation of N-nitrosamine in heated cured pork meat

The influence of biogenic amines (i.e. putrescine, cadaverine, spermidine and spermine) on the N-nitrosamine formation in heated cured lean meat was studied in the presence or absence of sodium nitrite and at different meat processing temperatures. Experimental evidence was produced using gas chromatography with thermal energy analysis detection (GC–TEA). Concentration of N-nitrosamines was modelled as a function of the temperature and the nitrite concentration for two situations, i.e. presence or absence of added biogenic amines to the meat. The significance of the influence of the changing parameters was evaluated by ANOVA (Analysis of Variance).     

A simplified method for the determination of several fish drugs in edible fish and shrimp by high-performance liquid chromatography

A simplified HPLC method was used to recover antibiotic and antibacterial agents from 11 cultured fish and one shrimp. The average recoveries of oxytetracycline, oxolinic acid, miloxacin, and sulfamonomethoxine were 77, 92, 89 and 80%, respectively. The detection limit was 0.02–0.04 μg/g. We also examined the recovery of oxytetracycline and oxolinic acid used for cultured black tiger shrimp, which is a popular imported shrimp in Japan. To demonstrate the usefulness of this technique for detecting drug residues in cultured fish, the method was used to examine the muscle tissues of 12 commercial fish and shrimp obtained from several fish shops. No agents were found in any of the fish tested.     

Aliphatic secondary amines in meat and fish products and their analysis by high pressure liquid chromatography

A simple and reliable high pressure liquid chromatographic method for aliphatic secondary amines in foods has been developed. The method, which involves rapid extraction, derivatisation with dinitroflurobenzene and one-step liquid chromatographic analysis, allows dimethylamine to be determined without interference by the completing agent, whereas only a slight increase in the response of dimethylamine is caused by large amounts of trimethylamine. The presence of free secondary amines in a number of Italian meat and fish products and their formation as a consequence of some preservation techniques have been investigated. The results are discussed.     

The determination of the component oligosaccharides of lupinseeds by high pressure liquid chromatography

A simple rapid method is reported for the analysis of oligosaccharides in lupinseeds. The procedure involves extraction of the ground, defatted seeds with aqueous methanol, precipitation of protein with Carrez solution and subsequent analysis using high pressure liquid chromatography. The chromatographic separation utilises Spherisorb amino columns (five micron) packed in our laboratory. Quantification is achieved by direct comparison with aqueous standards. The oligosaccharide composition of ten lupinseed varieties, from four species, are reported and the values obtained compared with those found for soy beans. The contents of stachyose and verbascose, which are considered to be of major importance as flatus factors, are found to be similar to those in soy beans for some lupinseed species (L. albus and L. angustifolius) but considerably higher in others (L. luteus and L. mutabilis).     

食品中马来酸的高压液相色谱法检测研究

目的 探讨应用高压液相色谱法来检测各种食品中的马来酸。方法 以Agilent SB C18色谱柱为分析柱, 确立了对淀粉、改性淀粉、蛋酥饼干、芋泥汤圆、刀削面、粉丝等食品中马来酸的高压液相色谱检测法。通过试验, 考察了富马酸对这些食品中的马来酸检测的影响。结果 在试验条件下, 富马酸不会对马来酸的检测造成影响。通过对方法的回收率和精密度进行分析探讨, 结果在所确定的实验条件下, 即流动相: 0.1 mol/L 磷酸二氢铵溶液(pH调至2.5), 流速: 0.6 mL/min, 检测波长: 240 nm, 柱温: 30℃, 峰面积和标准溶液在0.5~ 20.0 mg/L范围内呈良好线性关系, 线性系数大于0.999, 平均回收率处于93.8%~101.1%, RSD均小于5.0 %。结论 本实验方法安全可靠, 可以满足实际检测的需要。     

A high performance liquid chromatography method for determination of furfural in crude palm oil

A modified steam distillation method was developed to extract furfural from crude palm oil (CPO). The collected distillates were analysed using high performance liquid chromatography (HPLC) coupled with an ultraviolet diode detector at 284 nm. The HPLC method allowed identification and quantification of furfural in CPO. The unique thermal extraction of CPO whereby the fresh fruit bunches (FFB) are first subjected to steam treatment, distinguishes itself from other solvent-extracted or cold-pressed vegetable oils. The presence of furfural was also determined in the fresh palm oil from FFB (without undergoing the normal extraction process), palm olein, palm stearin, olive oil, coconut oil, sunflower oil, soya oil and corn oil. The chromatograms of the extracts were compared to that of standard furfural. Furfural was only detected in CPO. The CPO consignments obtained from four mills were shown to contain 7.54 to 20.60 mg/kg furfural.     

分光光度法测定鱼罐头中组胺的方法改进

在GB/T 5009.45-2003国家标准方法的基础上对样品的前处理等过程进行了新的尝试,使样品前处理过程简单、快速,同时保证了方法的准确度和精密度.结果显示,在60℃水浴、30 min条件下,三氯乙酸的提取效果最佳;正戊醇提取过程采用旋涡后离心的方式代替了分液漏斗振摇,获得了较佳的提取效果;盐酸提取液改为1.0 mL,保证了标准系列与测定系列显色体系的一致性,同时保证了实验结果的准确度.     

高效液相色谱法测定饮料中三氯蔗糖的含量的优化

目的优化高效液相色谱法(high performance liquid chromatography,HPLC)检测饮料中三氯蔗糖的含量。方法采用配备示差折光检测器的高效液相色谱仪,使用C18反相色谱柱,选择甲醇:0.125%磷酸氢二钾=40:60(V:V)作为流动相,在0.8 m L/min的流速下进行检测。结果该方法在20~400 mg/L范围内,三氯蔗糖的浓度与峰面积的相关性良好,标准曲线为Y=207.99X+274.1,r=0.9999,改进后方法回收率在94.28%~107.16%之间,改进后检出限为0.0024 g/kg。结论该方法不仅能够达到国家标准的要求,并且快速、灵敏、环保,提高了高效液相色谱检测饮料中三氯蔗糖的检测效率和安全性。     

A rapid method for the simultaneous determination of 25 anti-hypertensive compounds in dietary supplements using ultra-high-pressure liquid chromatography

A novel, stable, simple and specific ultra-performance liquid chromatography method with ultraviolet detection (205 nm) for the simultaneous analysis of 25 anti-hypertensive substances was developed. The method was validated according to the International Conference of Harmonisation guidelines with respect to linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ) and stability. From the ultra-performance liquid chromatography results, we identified the LOD and LOQ of solid samples to be 0.20–1.00 and 0.60–3.00 μg ml^?1, respectively, while those of liquid samples were 0.30–1.20 and 0.90–3.60 μg ml^?1, respectively. The linearity exceeded 0.9999, and the intra- and inter-day precisions were 0.15–6.48% and 0.28–8.67%, respectively. The intra- and inter-day accuracies were 82.25–111.42% and 80.70–115.64%, respectively, and the stability was lower than 12.9% (relative standard deviation). This method was applied to the monitoring of 97 commercially available dietary supplements obtained in Korea, such as pills, soft capsules, hard capsules, liquids, powders and tablets. The proposed method is accurate, precise and of high quality, and can be used for the routine, reproducible analysis and control of 25 anti-hypertensive substances in various dietary supplements. The work presented herein may help to prevent incidents related to food adulteration and restrict the illegal food market.     

高效液相色谱法测定乳制品中纳他霉素分析方法的改进

目的优化高效液相色谱法(high performance liquid chromatography,HPLC)测定乳制品中纳他霉素含量的分析方法。方法对测定纳他霉素GB/T 21915-2008《食品中纳他霉素的测定》的高效液相色谱法中样品的提取溶剂、蛋白沉淀剂、色谱流动相及流速进行优化,并对优化后的方法进行方法学验证。结果选择10%的冰乙酸水溶液作为样品提取溶剂;乙酸锌和亚铁氰化钾作为蛋白沉淀剂;甲醇-水-冰乙酸(60:40:2,V:V:V)作为流动相;流速为1.0 mL/min。可以在7 min内完成对目标物的分离,线性方程为Y=43315X-1751,r~2=0.99997,方法平均回收率在98.5%~106.3%之间,相对标准偏差(relative standard deviation,RSD)均小于2.2%,方法检出限为0.02 mg/L。结论该方法前处理简单,回收率及灵敏度高,准确度和稳定性好,适用于对纯牛奶、乳酸菌饮料、奶粉等乳制品中纳他霉素的分离和定量检测。     

Analysis of vitamin A in eggs by high pressure liquid chromatography

A high speed liquid chromatographic method was described for the rapid determination of vitamin A in eggs. After saponification and extraction, the sample was separated on a reversed-phase column (C18) with acetonitrile - methylene-chloride - methanol as the mobile phase. Quantitative determination was accomplished by monitoring the ultraviolet absorbance of retinol at 280 nm. Recovery of vitamin A was 97.1 %.     

高压液相色谱法快速测定饮料中的五种食品添加剂

目的 建立一种高压液相色谱方法同时检测饮料制品中3种甜味剂(安赛蜜、糖精钠、阿斯巴甜)和2种防腐剂(苯甲酸、山梨酸)。方法 样品采用起始流动相稀释后直接过膜分析, 色谱分离在极性修饰XAqua C18色谱柱上进行, 流动相采用50 mmol/L pH 4.5 KH2PO4和乙腈, 梯度模式洗脱, 流速2 mL/min, 柱温40 ℃, 6 min内即可完成一次分离分析, 加上4 min梯度平衡时间, 10 min内即可完成平衡及分离。结果 5种食品添加剂在0.5~50 mg/L内线性关系良好, 相关系数r2均大于0.9999。在两种饮料基质中添加50、100、150 mg/kg 3个浓度水平, 方法回收率为96.48%~105.64%, 相对标准偏差为0.21%~5.39%; 以信噪比S/N =3计算, 方法检测限为0.02~0.08 mg/L。结论 建立的分析方法快速、准确, 可满足饮料中甜味剂和防腐剂的同时检测。     

高效液相色谱法同时测定保健食品中红景天苷和腺苷

目的 建立同时测定保健食品中的红景天苷和腺苷含量的高效液相色谱测定方法.方法 采用50％甲醇为溶剂,超声提取样品中的的红景天苷和腺苷成分.采用shim-pack CLS-ODS色谱柱(150 mm ×4.6 mm,5μm),流动相为甲醇+ 20 mmol/L磷酸二氢钾水溶液(15 +85,V/V),流速1.0 ml/min,进样量10 μl,紫外检测波长为红景天苷275 nm,腺苷260 nm.结果 红景天苷在10.0 ～200 μg/ml范围内线性良好(r=0.999 5),平均回收率92.5％～99.5％,精密度2.8％～4.7％(n=6);腺苷在2.50～50.0μg/ml范围内线性良好(r=0.999 6),平均回收率90.0％～ 94.0％,精密度2.1％～5.2％(n=6).红景天苷和腺苷检出限LOD分别为0.01和0.005μ g/g.结论 本方法快捷、简便、灵敏度高,可准确同时测定保健食品中的红景天苷和腺苷含量.     

高效液相色谱法测定酱油中组胺的含量

目的 建立丹磺酰氯柱前衍生-高效液相色谱法测定酱油中组胺含量的方法.方法 样品酱油以1,7-二氨基庚烷作为内标,用正丁醇:三氯甲烷(1:1,V:V)萃取净化,经丹磺酰氯衍生,乙醚萃取后氮气吹干,用乙腈定容,高效液相色谱仪测定,内标法定量.结果 组胺含量在1～100 mg/L线性关系良好,线性相关系数r=0.9999,检...     

食品中低聚异麦芽糖高效液柑色谱检测方法研究

针对乳制品、固体饮料、糖果、保健品等食品中添加的功能活性成分低聚异麦芽糖,包括异麦芽糖(IG2)、潘糖(P)、异麦芽三糖(IG3)、异麦芽四糖(IG4)的检测,建立了水和乙腈为流动相,梯度洗脱,氨基色谱柱分离,蒸发光散射检测器(evaporative light-scattering detector,ELSD)检测食品中添加的低聚异麦芽糖舍量的高效波相色谱方法.异麦芽糖、潘糖、异麦芽三糖、异麦芽四糖的线性工作范围分别为0.1～0.45mg/mL、0.1～0.45mg/mL、0.2～0.65mg/mL、0.1～0.35mg/mL,线性相关系数R2分别为1、0.9999、0.9998、0.9999.对不同类型的食品,四种低聚异麦芽糖的回收率在98.0%～105.0%之间.方法准确度高.室内重复性变异系数一般都低于10%;除了含量低的异麦芽四糖,室间再现性变异系数一般都低于10%,说明方法的重复性和再现性良好.该方法简单、易于掌握,测定结果准确,适于复杂食品基质中低聚异麦芽糖含量的测定.     

Extended liquid chromatography high resolution mass spectrometry screening method for veterinary drug,pesticide and human pharmaceutical residues in aquaculture fish

ABSTRACT

A liquid chromatography high resolution mass spectrometry (LC-HRMS) screening method was developed previously to analyze for veterinary drug residues commonly found in different types of aquaculture products. This method has been further evaluated for its feasibility to detect several other classes of compounds that might also be a concern as possible contaminants in farmed tilapia, salmon, eel and shrimp. Some chemicals could contaminate water sources used in aquaculture production through agricultural run-off. These compounds include several widely used triazine herbicides, organophosphate and carbamate pesticides, as well as various discarded human pharmaceuticals. Other possible contaminants investigated were selected disinfectants, some newer antibiotics, growth promoters, and various parasiticides. The sample preparation consisted of an acidic acetonitrile extraction followed by solid-phase extraction clean-up. Data were collected with a quadrupole-Orbitrap MS using both non-targeted and targeted acquisition. This rapid clean-up procedure and HRMS detection method described previously for veterinary drug residues also worked well for many other types of compounds. Most analytes had screening limit levels between 0.5–10 ng/g in the matrices examined using exact mass identification criteria. The strategy described in this paper for testing the performance of additional analytes will help expand the applicability of the HRMS procedure as aquaculture samples can now be analyzed for a wider range of contaminants.     

高效液相色谱法测定乳粉中维生素E方法的优化

目的优化GB5009.82-2016《食品安全国家标准食品中维生素A、D、E的测定》中高效液相色谱法测定维生素E的样品制备和色谱分析条件。方法样品经乙醇-氢氧化钾水浴皂化后,石油醚-乙醚萃取,氮吹至尽干,甲醇溶解幵过滤,采用甲醇:四氢呋喃=99:1(V:V)作为流动相进行等度洗脱,外标法定量。结果本方法在10 min内完成维生素E的4种异构体的分离分析,精密度、线性良好。4种异构体在0.5、15和40μg/m L添加水平的回收率为96.1%~101.2%,维生素E的相对标准偏差小于1.7%(n=10),方法定量限为100μg/100g。结论优化后的方法快速、准确、灵敏,适合乳粉中维生素E异构体的快速准确测定。     

高效液相色谱法测定鱼油软胶囊中维生素D3含量的不确定度评定

目的评定高效液相色谱法(high performance liquid chromatography,HPLC)测定鱼油软胶囊中维生素D_3含量的不确定度。方法依据国家计量技术规范JJF 1059.1-2012《测量不确定度评定与表示》对维生素D_3测定中的不确定度来源进行分析。通过建立数学模型量化不确定度分量,计算合成不确定度和扩展不确定度。结果本方法的不确定度主要来源于标准物质的含量、标准曲线的配制和标准曲线的拟合。当样品中维生素D_3的含量为2.08μg/kg,扩展不确定度为0.20μg/kg,维生素D_3含量表示为(2.08±0.20)μg/kg(k=2)。结论该评定方法可用于高效液相色谱法对鱼油软胶囊中维生素D_3的不确定分析。     

Validation of a high performance liquid chromatography method for sunscreen determination in cosmetics

The aim of this research was the development and validation of a high performance liquid chromatography (HPLC) method for the simultaneous and quantitative determination of benzophenone-3, octyl methoxycinnamate and octyl salicylate contained in sunscreen emulsions. The separation and quantitative determination was achieved using a LiChrospher((R)) 100 RP-18 (5 microm) Merck column, a mobile phase constituted of methanol/water (85/15, v/v), a flow-rate of 1.0 mL min(-1) and UV detection at 310 nm. The correlation coefficients and percentage of recovery for benzophenone-3, octyl methoxycinnamate and octyl salicylate were 0.9999 and 99.46%; 0.9995 and 98.85%; 0.9998 and 98.84%, respectively. The relative standard deviations (RSD) for commercial samples were between 0.50 and 0.70%.     

食品中低聚果糖高效液相色谱检测方法研究

针对乳制品、糕点、酒类、饮料、糖果等食品中添加的功能活性成分低聚果糖,包括蔗果三糖(GF2)、蔗果四糖(GF3)、蔗果五糖(GF4)的检测,建立了水和乙腈为流动相,梯度洗脱,氨基色谱柱分离,蒸发光散射检测器(evaporativelight-scattering detector,ELSD)检测食品中添加的低聚果糖含量的高效液相色谱方法。蔗果三糖、蔗果四糖、蔗果五糖的线性工作范围分别为0·04~0·45、0·05~0·50、0·04~0·45mg/mL,线性相关系数R2分别为0·9999、0·9999、1。对不同类型的食品,三种低聚果糖的回收率在90·0%~110·0%之间,方法准确度高。室内重复性变异系数一般都低于10%,室间再现性变异系数一般都低于15%,说明方法的重复性和再现性良好。该方法简单、易于掌握,测定结果准确,适于复杂食品基质中低聚果糖含量的测定。