高效液相色谱-蒸发光散射检测法同时测定食品中9种甜味剂

目的建立高效液相色谱-蒸发光散射检测器(high performance liquid chromatography-evaporative light scattering detection,HPLC-ELSD)同时检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、索马甜、纽甜、甜菊糖苷9种甜味剂的方法。方法样品中的甜味剂经水提取后利用固相萃取柱净化浓缩,以C_18(250 mm×4.6 mm,5μm)柱分离,经流动相梯度洗脱后,采用HPLC-ELSD法进行测定。结果 9种甜味剂在20~500 mg/L的质量浓度范围内,具有良好的线性关系(相关系数大于0.99),在3个添加水平下样品的平均回收率为87.2%~107.1%,相对标准偏差小于4.0%,该方法中三氯蔗糖、阿斯巴甜、阿力甜、索马甜、纽甜和甜菊糖苷的检出限为5 mg/kg,安赛蜜、糖精钠和甜蜜素的检出限为10 mg/kg。结论本方法简单、准确、灵敏,是同时检测食品中9种甜味剂的有效方法。     

超高压液相色谱—质谱同时测定白酒中6种微量甜味剂的方法研究

为了检测白酒中6种甜味剂(安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、纽甜),建立了一种超高压液相色谱质谱联用的新方法。样品预处理后,通过BEH C-18色谱柱分离,以甲醇-20 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在ESI负离子模式下检测,一次进样分析仅需10 min。以优化后的条件进行测定,6种甜味剂线性范围均在0.05~5.0 mg/L内,线性相关系数均大于0.994 5。得到安赛蜜检出限为0.05 mg/L、糖精钠、甜蜜素、纽甜检出限为0.01 mg/L、三氯蔗糖、阿斯巴甜检出限为0.1 mg/L。加标水平为0.5 mg/L和1.0 mg/L时,回收率在86.48%~116.90%之间,相对标准偏差为0.22%-3.90%。方法准确可靠、简便快速、可达到同时检测6种甜味剂的目的。     

高效液相色谱法检测酸牛乳中纳他霉素含量的几种前处理方法比较

在酸牛乳基质中分别添加0．64mg／L、1．28mg／L、3．2mg／L、6．4mg／L、12．8mg／L5个浓度的纳他霉素标准品。分别用几种方法进行了酸牛乳样品前处理，高效液相色谱仪测定，外标法定量。比较了几种方法的回收率、检出限及通过滤膜难易程度。结果表明：方法的回收率为66％。103％，检出限为0．02mg／kg-0．03mg／kg。     

离子排斥色谱法、脉冲安培检测器对食品中亚硫酸及其盐的分析与检测

研究了离子排斥色谱法、脉冲安培检测器分析检测亚硫酸根的方法，检出限为2．89mg／L，相对标准偏差为2．7％，线性相关系数为0．9910。该方法用于食品样品的分析，结果令人满意。     

微波程序消解-流动注射化学发光法快速测定彩色小麦中的微量铬

为了建立一种快速测定小麦中微量铬的新方法,以南阳彩色小麦粉为样品,经微波程序消解后,用亚硫酸将高价铬还原为Cr3＋,利用Cr3＋对Lumin01．H202化学发光体系的线性催化作用测定南阳彩色小麦中的总铬含量。结果表明：样品中的铬含量为2．211～6．088mg／kg,线性相关系数r=-0．9988,对5．0×10^-8mol／L Cr3＋测定的RSD为4．5％（n=11）,按3倍标准偏差（3S）计算的检出限为3．75×10^-11mol／L,灰麦加标回收率为93．66％~99．09％。该法快速简便、灵敏度高、选择性好,用于彩色小麦中微量铬的测定,结果令人满意。     

固相萃取-高效液相色谱法测定酱油中的7种有机酸

提出了一种利用固相萃取．高效液相色谱法同时分析酱油中焦谷氨酸等7种有机酸的方法。酱油经制样后过StrataSAX固相萃取（SPE）小柱净化,在AgilentSB-Aq（150mm×4．6mm×5μm）色谱柱上,0．01mol／L磷酸氢二铵（pH2．7）溶液为流动相,流速为0．7mL／min,柱温为35℃,紫外检测波长为210mm时,可以较好地分离和测定酱油中焦谷氨酸等7种有机酸。该方法相对标准偏差0．13%-1．9％,回收率95．0％-105％,各种酸的线性相关系数r〉0．9993,具有较高的准确度和精密度,方法简便,可应用于酱油中有机酸的检测。     

用高效液相色谱法同时测定葡萄酒中4种色素含量方法的研究

为了建立同时测定葡萄酒中喹啉黄、坚牢绿、偶氮玉红（又名酸性红,二蓝光酸性红）和专利蓝等4种色素含量的高效液相色谱方法,采用样品除去乙醇,经水提取和过滤后,使用C18色谱柱（4．6×250mm,5μm）分离,以甲醇和乙酸铵（0．02mol／L）为流动相梯度洗脱,流速为1．0mL／min,二极管阵列检测器检测,波长410nm,柱温30℃。结果显示：4种色素的工作曲线在1．0～50．0μg／mL范围内浓度与峰面积呈良好的线性关系,相关系数r均〉0．999。以S／N=3确定各检出限：喹啉黄为0．23mg／kg,坚牢绿为0．37mg／kg,偶氮玉红为0．29mg／kg,专利蓝为0．15mg／kg。精密度（RSD,n=6）〈3．0％。回收率在91．5％～100．8％。说明该方法干扰小,灵敏度高,分离效果好,操作简便、快速和准确可靠。     

反相液相色谱同时测定糖品中的防腐剂和甜味剂

本文建立了用反相液相色谱同时测定糖品中的苯甲酸、山梨酸、脱氢乙酸、安赛蜜、糖精钠等防腐剂和甜味剂的方法。方法采用VenusilXBP—C18（5gm,4．6x250mm）反相色谱柱,流动相为20mmol／L乙酸铵一甲醇,流速为1．0mL／min,柱温为30℃,进样量为10gL。该方法的测定低限为1．0mg／L,线性范围为10～100mg／L,加标回收率为89．85％～103．60％,相对标准偏差为1．50％～3．26％（n=4）。结果表明,该方法简便、可靠,适合对糖品中防腐剂和甜味剂的同时检测。     

离子色谱法测定米粉、米线、河粉、粉丝中的亚硫酸盐

利用离子交换-电导检测离子色谱法测定米粉、河粉、粉丝中的亚硫酸盐含量,选用IonPac AS11型分离柱,4．5mmol／L NaOH为淋洗液,加电自动抑制模式,此方法的相关性好（r=0.9998）。样品加标平均回收率为89．12％-92．07％,检出限为0．057mg／L。该方法准确度高,重现性好,操作简便。     

食品中丙烯酰胺含量的分析方法研究

富含淀粉类食品经高温烹饪会产生较高浓度的丙烯酰胺。丙烯酰胺是一种对人类可能的致癌物质。本文建立了用气相色谱-质谱直接测定食品中丙烯酰胺含量的方法。采用选择离了采集模式，方法的线性范围是0．5～15．5mg／L，线性相关系数为r=0．99943，回收率在94％以上，相对标准偏差小于5．4％，定量检测限25μg／kg。是一种快速、灵敏的测定方法。     

超高效液相色谱法测定焙烤食品中9种甜味剂及防腐剂

目的建立超高效液相色谱法(ultra performance liquid chromatography, UPLC)检测焙烤食品如面包、蛋糕及饼干中9种甜味剂及防腐剂的分析方法。方法样品经水提取,乙酸锌、亚铁氰化钾沉淀蛋白,正己烷除脂后,经UPLC二极管阵列检测器检测。结果 9种添加剂在范围内线性关系良好,相关系数均大于0.9999;方法回收率为74.3%~125.4%,相对标准偏差(relative standard deviation, RSD)为1.92%~9.09%;安赛蜜、苯甲酸、山梨酸、脱氢乙酸、糖精钠、水杨酸检出限为1.5 mg/kg;阿斯巴甜、阿力甜、纽甜检出限为3.0 mg/kg。结论该方法操作简单快速、重现性好,可用于面包、蛋糕及饼干中9种甜味剂及防腐剂的检测。     

UPLC-MS/MS同时测定电子烟烟液中安赛蜜等5种合成甜味剂

  目的  通过对实验条件的优化,建立了一种测定电子烟烟液中5种人工合成甜味剂（安赛蜜、甜蜜素、糖精钠、阿斯巴甜和纽甜）的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。  方法  样品经超纯水稀释、C₁₈分散固相萃取净化后,以BEH C₁₈色谱柱分离,甲醇-0.1%甲酸水溶液为流动相,外标法定量。  结果  结果表明:①5种甜味剂在0.25~5.0 μg/mL的标准工作曲线范围内线性关系良好（r > 0.998）,检出限（LOD）和定量限（LOQ）分别为0.02~0.05和0.07~0.17 mg·kg-1,回收率为92.5%~105.2%,相对标准偏差（RSDs）＜5.0%。②采用该方法对10个电子烟烟液样品进行了检测,1个样品检出甜蜜素,含量为2.48 mg·kg-1,2个样品检出纽甜,含量在3.35~4.52 mg·kg-1之间。  结论  该方法操作简单、快速、灵敏度高、有机溶剂消耗少,适用于电子烟烟液中多种甜味剂的同时检测。      

Saccharin and other artificial sweeteners in soils: estimated inputs from agriculture and households, degradation, and leaching to groundwater

Artificial sweeteners are consumed in substantial quantities as sugar substitutes and were previously shown to be ubiquitously present in the aquatic environment. The sweetener saccharin is also registered as additive in piglet feed. Saccharin fed to piglets was largely excreted and, consequently, found in liquid manure at concentrations up to 12 mg/L, where it was stable during 2 months of storage. Saccharin may thus end up in soils in considerable quantities with manure. Furthermore, other studies showed that saccharin is a soil metabolite of certain sulfonylurea herbicides. Sweeteners may also get into soils via irrigation with wastewater-polluted surface water, fertilization with sewage sludge (1-43 μg/L), or through leaky sewers. In soil incubation experiments, cyclamate, saccharin, acesulfame, and sucralose were degraded with half-lives of 0.4-6 d, 3-12 d, 3-49 d, and 8-124 d, respectively. The relative importance of entry pathways to soils was compared and degradation and leaching to groundwater were evaluated with computer simulations. The data suggest that detection of saccharin in groundwater (observed concentrations, up to 0.26 μg/L) is most likely due to application of manure. However, elevated concentrations of acesulfame in groundwater (up to 5 μg/L) may result primarily from infiltration of wastewater-polluted surface water through stream beds.     

Monitoring sweetener consumption in Great Britain.

A comprehensive survey of the consumption of intense sweeteners in Great Britain in 1988 quantified the levels of usage of different sweeteners and identified their distribution between food categories and population subgroups. Saccharin was found to be the most widely used intense sweetener. Beverages were the most common source of intense sweeteners. The quantities consumed of all sweeteners were found to be below the Acceptable Daily Intake (ADI) values established by the Joint FAO/WHO Expert Committee on Food Additives, the European Commission Scientific Committee for Food or the UK Committee on Toxicity of Chemicals in Food, Consumer Products and the Environment.     

甜味剂和苯甲酸在涂覆型整体柱上的快速测定

结合甜味剂具有紫外吸收的特点,以涂覆阳离子表面活性剂(氯代十六烷基吡啶)的整体柱为分离柱,采用紫外检测的方法,测定了包括安赛蜜、阿斯巴甜和糖精钠在内的3种常见的甜味剂以及常用的防腐剂苯甲酸。在最佳的色谱条件下,这几种物质都具有很好的线性关系和重复性。可以在120s内完成以上4种物质的分离。以满足饮料、药品等多种实际样品进行快速测定甜味剂和防腐剂的需要。     

Headspace solid-phase micro-extraction gas chromatography method for the determination of methanol in aspartame sweeteners

A headspace solid-phase micro-extraction (HS-SPME) method for the extraction and determination of residual methanol in artificial sweeteners by capillary gas chromatography with flame ionization detection (GC-FID) is described. A manual SPME holder with an 85-µm polyacrylate fibre was used. The optimized conditions for methanol extraction by SPME were: sample agitation, absorption temperature of 30°C, absorption time of 10 min, desorption time of 2 min and sample volume in the vial of 400.0 µl. Under these conditions the calibration graphs were linear in the range 2.50-31.60 mg l^-1, and the precision was good (relative standard deviation 4.9%). The detection limit was 0.40 mg l^-1; the quantification limit was 2.06 mg l^-1.     

微波提取-高效液相色谱法同时测定月饼中的5种防腐剂和甜味剂

该研究建立了微波提取-高效液相色谱法同时测定月饼中的5种防腐剂和甜味剂的分析方法,研究了流动相和检测波长,设计正交试验优化了微波提取的条件,并对比了微波提取和超声提取的效果。结果显示微波提取在提取效率上更有优势,提取时间只需要超声提取时间的1/15。该分析方法检出限为0.2mg/kg～0.70mg/kg,线性范围为0.4mg/L～400mg/L,加标回收率为96.0%～103.2%,满足分析检测的要求。     

白酒中甜味剂的检测及其来源的探讨

建立了白酒中4种甜味剂（安赛蜜、甜蜜素、糖精钠、三氯蔗糖）的高效液相色谱-串联质谱的检测方法。采用Agilent EC-C18色谱柱,以甲醇-乙酸铵溶液为流动相,柱温35 ℃,流速0.8 mL/min梯度洗脱进行检测。结果表明,4种甜味剂在5～100 ng/mL范围内呈良好线性关系（相关系数R2≥0.998 6）,检出限为0.001～0.02 mg/kg,回收率在82.70%～117.62%之间,相对标准偏差（RSD）为1.09%～4.64%。该检测方法快速灵敏,大大缩短了检测周期和检测成本,并通过大量样品的检测对白酒中甜味剂的来源进行了探讨。     

HPLC-MS/MS analysis of 9 artificial sweeteners in imported foods

An analytical method for the simultaneous determination of 9 artificial sweeteners (acesulfame-K, cyclamate, sodium saccharin, aspartame, alitame, neotame, sucralose, dulcin, and neohesperidine dihydrochalcone) in imported foods by HPLC-MS/MS was developed. Samples were extracted with buffer solution (pH 4.5). The supernatant was analyzed by HPLC-MS/MS after centrifugation and filtration. The sample was separated on a thermo hypersil BPS C₁₈ (250×3 mm, 5-μm) column, and detected by MS/MS with selective reaction monitoring (SRM) mode. The correlation coefficients (r ²) of the calibration curve were >0.99. The recoveries were 90.0–107.5% with good coefficients of variation of 1.8–8.6%. The limits of detection and limits of quantification were between 0.001 and 0.375 mg/mL and between 0.003 and 1.125 mg/mL, respectively. The proposed method has been successfully applied to the determination of the 9 sweeteners in various foods.

     

微波消解—ICP-MS法测定坚果和果蔬籽仁中As、Pb、Hg、Mg、Al含量

为了建立密闭式微波消解—ICP-MS法同时测定坚果与果蔬籽仁中As、Pb、Hg、Mg、Al含量的方法。采用微波消解仪对坚果与果蔬籽仁样品进行密闭消解,然后用电感耦合等离子体质谱分析仪,以~(72)Ge作为As的内标、~(209)Bi作为Pb和Hg的内标、~(45)Sc作为Mg和Al的内标控制分析信号的动态漂移,对坚果与果蔬籽仁中的As、Pb、Hg、Mg、Al进行同时测定。结果表明:As、Pb、Hg、Mg、Al的回收率在95%~105%之间;As、Pb、Hg、Mg、Al的检出限分别为0.005、0.005、0.001、0.01、0.005 mg/kg;线性相关系数均大于0.999 9;相对标准偏差(RSD)均小于2%。同时对国家标准物质大米进行分析,结果测定值在标准值范围内。本法回收率、检出限、准确度、精密度试验的结果均满足要求,可用于测定坚果与果蔬籽仁中As、Pb、Hg、Mg、Al含量,并为完善坚果与果蔬籽仁质量标准提供依据。