紫外可见分光光度法检测蛋黄中微量苏丹红Ⅳ

本实验建立了紫外可见分光光度法检测蛋黄中微量苏丹红Ⅳ的新方法,蛋黄样品经过预处理后利用紫外-可见光检测器测定吸光度,并用外标法分析定量。当苏丹红Ⅳ在1～12μg/mL时,其特征峰的吸光值与苏丹红Ⅳ含量呈良好线性性关系。运用于蛋黄实际样品检测,其加标回收率为97%～105%,检出限低至0.05μg/mL,测定结果与其他方法比对无显著差异。该方法具有简单、快速、准确度高等特点,能运用于蛋黄中微量苏丹红Ⅳ的快速测定。     

辣椒制品中的苏丹红检测方法的优化

优化了辣椒及其制品中苏丹红Ⅰ~Ⅳ的检测方法。样品经固相萃取净化后,以乙腈和0.75%的乙酸水为流动相,梯度洗脱,经C18柱分离,于500nm波长下检测。结果表明:苏丹红Ⅰ~Ⅳ在0.08~2.56μg/mL时有良好的线性关系,在添加浓度为0.15~1.28μg/mL时,辣椒粉中苏丹红Ⅰ~Ⅳ回收率为86.2%~97.7%;辣椒油中苏丹红Ⅰ~Ⅳ回收率为87.2%~94.8%;辣椒酱中苏丹红Ⅰ~Ⅳ回收率为82.7%~92.0%。苏丹红Ⅰ~Ⅳ的检出限分别为0.03,0.05,0.03,0.06μg/mL。实验表明:优化后的方法比国标GB/T 19681-2005方法耗时短,灵敏度高,简便,重现性好,适于实验室的日常检测。     

固相萃取-HPLC法测定辣椒油中偶氮染料

建立一种基于大孔吸附树脂柱对辣椒油中苏丹红Ⅰ-Ⅳ、苏丹红7B和对位红等6种偶氮染料进行的前处理方法。辣椒油样品经正己烷稀释,用自制大孔吸附树脂柱净化,用高效液相色谱-二极管阵列检测器检测,自制固相萃取柱经再生过程可重复使用。结果显示,6种染料在0.05μg/mL~1.0μg/mL浓度范围内线性关系良好,相关系数高于0.999 8,在3个加标浓度下,日内和日间的加标回收率在90.9%~104.3%之间,相对标准偏差(RSD)小于3.7%。     

HPLC法同时检测辣椒制品中8种非食用红色色素

建立了凝胶柱净化-高效液相色谱法同时检测辣椒制品中苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、对位红、苏丹红G、苏丹红7B和苏丹红B等8种红色色素的方法。样品用正己烷或正己烷/丙酮提取,提取液经BioBeadsS-X3凝胶柱净化。净化后的样品采用ZorbaxSBC18柱分离,以0.1%甲酸水溶液(A)和含0.1%甲酸的甲醇丙酮(9∶1,V/V)溶液(B)为流动相,流速1mL/min,检测波长505nm。上述8种色素组分在其质量浓度为0.16～2.56mg/L时有良好的线性关系,方法的检测限为15～46μg/kg;平均加标回收率为89.9%～118.2%,相对标准偏差为2.3%～4.8%。该方法灵敏可靠,适合于辣椒制品中多种脂溶性红色色素的同时检测。     

高效液相色谱测定食品中非食用色素丽春红2R的含量

为建立食品中非食用色素丽春红2R的高效液相色谱定量检测方法,样品经乙醇-氨水提取,以乙腈-5 mmol/L乙酸铵+0.06%三乙胺水溶液为流动相,XDB-C18色谱柱分离,二极管阵列检测器检测,检测波长为504 nm,外标法定量分析辣椒粉中的丽春红2R的含量.该方法线性范围为0.5μg/mL～15 μg/mL,最低检出浓度为0.02mg/L,RSD为1.32%～1.96%,加标平均回收率为96.19%.     

超高效液相色谱-质谱联用法(UPLC-MS/MS)测定辣椒制品中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ的含量

建立简便快速的测定辣椒制品中4种苏丹红染料的检测方法,以乙腈为提取溶剂,采用乙腈-0.1%水溶液的流动相体系和正离子电离模式,用UPLC-MS/MS测定4种苏丹红染料;苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ线性范围为0～200ng/mL,R2大于0.9911,检出限分别为1.0、2.0、2.0、4.0μg/kg,加标回收率均大于75%,RSD小于10%。该方法简便灵敏,准确快速,可用于辣椒制品中4种苏丹红染料的测定及确证。     

超高效液相色谱-串联质谱法测定禽蛋中 苏丹红的残留量

目的建立禽蛋中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ染料残留的液相色谱-串联质谱的检测方法。方法禽蛋样品中的苏丹红经溶解、冷冻离心及过滤提取纯化,经ZorbaxSB-C_(18)(2.1 mm×50 mm, 3.5μm)色谱柱,以乙腈和0.2%的甲酸水溶液为流动相进行等度洗脱,温度为35℃,流速为0.2mL/min,外标法定量。结果在1～50μg/kg的浓度范围内,线性关系良好(r0.99),样品中的检出限0.5μg/kg,分析时间仅为5 min,加标回收率为69.5%～108.2%,相对标准偏差为1.6%～17.5%。结论该方法准确、快速、灵敏度高,适用于禽蛋中苏丹红染料的测定。     

食品中苏丹红Ⅰ～Ⅳ检测方法的研究

目的在现用专项检测标准的基础上,优化一种合理、快速的基于高效液相色谱分离的测定苏丹红Ⅰ~Ⅳ的方法。方法探讨了提取溶剂、吸附剂、洗脱溶剂等对苏丹红分离的影响。结果在相同流动相和测定波长下,改进后的方法标准曲线线性非常好,r大于0.999 99,RSD为1.3%~1.5%,样品加标回收率为94.5%~109.4%。结论可用于苏丹红Ⅰ~Ⅳ的检测,具有灵敏度高、重现性好的特点。     

HPLC紫外检测法测定辣椒制品中苏丹红Ⅰ～Ⅳ号含量的研究

实验选用氟罗里硅土(FLORISIL)固相萃取(SPE)柱对样品进行净化,用DIKMA公司C18(150×4.6 mm,5μm)钻石柱为色谱柱,以含5%水的乙腈溶液为流动相,以229nm为检测波长,对辣椒食品中的苏丹红Ⅰ～Ⅳ号进行了分离和检测.结果显示:苏丹红Ⅰ～Ⅳ号分别在0.625～2000 ng、2.5～2000 ng、5～2000 ng、5～2000 ng范围内呈良好的线性关系,相关系数R2分别为1、1、0.9989和0.9990.其标准回收率分别为100.76%、100.20%、99.86%、100.09%,变异系数分别为1.04%、1.80%、3.29%、3.06%.辣椒粉样品中的苏丹红Ⅰ～Ⅳ号的加样回收率分别为102.14%、103.69%、96.36%和101.93%,变异系数分别为1.49%、0.84%、0.93%和3.64%;辣椒油样品中的苏丹红Ⅰ～Ⅳ号的加样回收率分别为97.03%、100.81%、94.53%和99.31%,变异系数分别为2.85%、1.71%、1.92%和2.79%.苏丹红Ⅰ～Ⅳ号的最低检测限分别为1.88、2.5、6.25和10μg/kg.该方法样品处理简单,灵敏度高,可在有关实验室推广应用.     

固相分散萃取-高效液相色谱法测定郫县豆瓣中四种苏丹红染料的研究

建立了郫县豆瓣中苏丹红Ⅰ～Ⅳ的固相分散萃取(SPDE)-高效液相色谱(HPLC)分析方法。样品用无水硫酸钠作为分散剂,以乙腈提取样品中的苏丹红,提取液用中性氧化铝层析柱进行净化。用Inertsil ODS-sp C18柱(4.6mm×250mm,5μm))分离,流动相A为乙腈,流动相B为0.1%甲酸水溶液(A∶B为90∶10,V/V),等度洗脱,流速1mL/min,柱温40℃。二极管阵列检测器检测,检测波长为517nm,利用保留时间和光谱图定性,外标法定量。4种苏丹红染料在0.10～20.00μg/mL范围内线性关系良好,相关系数均大于0.9999,苏丹红Ⅰ～Ⅳ的检出限(LOD)分别为0.009～0.013mg/kg(信噪比S/N=3)。在添加浓度为0.5～10.0mg/kg范围内平均回收率达81.67%～93.28%,相对标准偏差(RSD)为1.07%～4.61%(n=6)。     

基质固相分散术-UPLC 法检测禽蛋中对位红和苏丹红

建立禽蛋中对位红和苏丹红Ⅰ～Ⅳ号5 种色素的液相色谱检测方法。采用基质固相分散术,以氧化铝作基质分散基体,混合均匀的样品用正己烷- 丙酮(99.5:0.5,V/V)直接洗脱,吹干后定容测定,外标法定量。5 种色素的平均回收率为63.8%～96.2%,平均变异系数为0.52%～10.07%,检测限为0.01～0.02mg/kg。在检测的100个样品中,1 例检出苏丹红Ⅳ号。     

基质固相分散-高效液相色谱法测定川味香肠中的苏丹红染料

建立了川味香肠中苏丹红I～IV的基质固相分散(MSPD)-高效液相色谱(HPLC)分析方法。样品以无水硫酸钠作为分散基体,研磨均匀后与中性氧化铝同时装柱,正己烷淋洗净化,以丙酮-正己烷(5∶95,V/V)溶液洗脱。用InertsilODS-spC18柱(4.6mm×250mm,5μm)进行分离,流动相A为含0.1%甲酸的甲醇,流动相B为0.02mol/L的乙酸铵溶液(A∶B=85∶15,V/V),等度洗脱,柱温40℃。二极管阵列检测器检测,检测波长为490nm,利用保留时间和光谱图定性,外标法定量。4种苏丹红染料在0.10～50.00μg/mL范围内线性关系良好,相关系数均大于0.9999,苏丹红I、II、III、IV的检出限(LOD)分别为0.008～0.011mg/kg(信噪比S/N=3)。在添加浓度为5.0～25.0mg/kg范围内平均回收率达85.54%～94.66%,相对标准偏差(RSD)为0.87%～4.23%(n=6)。     

高效液相色谱法测定食品中可能掺杂的16 种工业染料

建立食品中16 种工业染料的高效液相色谱检测法,包括分散红11、分散黄9、分散橙3、分散橙11、分散红1、分散红9、分散黄54、分散橙37、分散橙61、苏丹红1、分散黄7、分散橙149、苏丹红2、苏丹红3、苏丹红7B、苏丹红4。选择糖果、巧克力、番茄酱与番茄沙司为基质,使用Agilent ZORBAX SB-C18色谱柱进行分离,流速为0.8 mL/min,流动相为乙腈和水,验证过程中确定检出限为0.26～0.88 mg/kg、定量限为0.82～2.52 mg/kg,16 种染料的回收率在81.0%～110.3%之间,相对标准偏差在0.3%～7.5%之间。表明方法稳定可靠,可用于日常的非法添加染料的测定和筛查。     

A simple and small-scale sample preparation technique to determine canthaxanthin in hen egg yolk

This paper describes an easy, small-scale method of sample preparation followed by a reversed-phase (RP) high-performance liquid chromatography (HPLC) for quantifying canthaxanthin (CX) in egg yolk. The egg yolk extract including CX was purified by using a normal-phase InterSep®-CN mini-syringe-column as a solid-phase extraction column. HPLC was performed on a C8 column with an isocratic mobile phase and diode array detector. The proposed method was validated by the analyses of spiked egg yolk samples; resulting recoveries (?94.5%; RSD ? 2.8%), analytical total time (<1 h/sample), and limit of quantitation (0.5 μg/g). The decision limit and detection capability were 25.04 and 25.07 μg/g, respectively.     

HPLC紫外检测法测定辣椒制品中苏丹红I～IV号含量的研究

实验选用氟罗里硅土(FLORISIL)固相萃取(SPE)柱对样品进行净化,用DIKMA公司C18(150×4.6mm,5μm)钻石柱为色谱柱,以含5%水的乙腈溶液为流动相,以229nm为检测波长,对辣椒食品中的苏丹红I～IV号进行了分离和检测。结果显示:苏丹红I～IV号分别在0.625～2000ng、2.5～2000ng、5～2000ng、5～2000ng范围内呈良好的线性关系,相关系数R2分别为1、1、0.9989和0.9990。其标准回收率分别为100.76%、100.20%、99.86%、100.09%,变异系数分别为1.04%、1.80%、3.29%、3.06%。辣椒粉样品中的苏丹红I～IV号的加样回收率分别为102.14%、103.69%、96.36%和101.93%,变异系数分别为1.49%、0.84%、0.93%和3.64%;辣椒油样品中的苏丹红I～IV号的加样回收率分别为97.03%、100.81%、94.53%和99.31%,变异系数分别为2.85%、1.71%、1.92%和2.79%。苏丹红I～IV号的最低检测限分别为1.88、2.5、6.25和10μg/kg。该方法样品处理简单,灵敏度高,可在有关实验室推广应用。     

AN IMPROVED METHOD OF CHOLESTEROL DETERMINATION IN EGG YOLK BY HPLC

An improved method for cholesterol determination in egg yolk is reported in this paper. Egg yolk was first diluted. Cholesterol was then extracted with ether and petroleum ether, and quantified by reverse phase chromatography on a Zorbax ODS column (0.46 × 15cm, 5–6 μm) using a mobile phase of acetonitrile and 2-propanol (4:1) with a flow rate of 0.6 mL/min. A linear correlation was observed between cholesterol concentration at 0.05–0.40 mg/mL and its peak heights with a correlation coefficient of 0.9993 (n = 5). The average recovery was 98.9%, and detection limit was 0.02 mg/mL. No differences in cholesterol concentration were observed between egg yolk samples with and without saponification. Rapid and reproducible quantification of cholesterol in egg yolk can be completed with this simplified method.     

HPLC法检测细胞培养上清液中前列腺素E2的含量

建立了检测巨噬细胞培养上清液前列腺素E2(PGE2)含量的高效液相色谱法,为检测体外细胞培养液PGE2提供快速定量的方法。色谱条件为:Ultimate XB-C18反相柱(250mm×4.6mm,5μm);以乙腈和0.02mol/L磷酸二氢钾水溶液(60∶40,v/v)作为流动相;流量为1mL/min;检测波长为196nm。结果表明:该方法标准曲线良好,线性范围为0.5625～90μg/mL,相关系数为R2=0.999,出峰时间为3.988min,最低检测限为0.1448μg/mL,平均回收率为100.71%。本方法简单快速,适用于样品数目较多的PGE2的快速定量检测。     

高效液相色谱示差折光法检测紫胶桐酸

采用高效液相色谱(high performance liquid chromatography,HPLC)法,利用示差折光检测器(refractive index detector ,RID)测定紫胶桐酸含量。色谱柱为Agilent ZORBAX SB-C18(4.6mm×250mm,5μm),以V(甲醇):V(水)＝60:40(0.1%三氟乙酸)作为流动相,流速1mL/min,进样体积10μL,柱温30℃。结果表明：紫胶桐酸在0.01～1.0mg/mL呈良好的线性关系,R2＝0.9994;最低检测限为0.008mg/mL;精密度RSD值为0.86%;平均加标回收率为100.23%,RSD值为0.65%。采用HPLC-RID测定紫胶桐酸的含量,操作简单,结果准确,稳定性和可信度好。     

A rapid HPLC method for determination of Sudan dyes and Para Red in red chilli pepper

A rapid high-performance liquid chromatography (HPLC) system consisting of an ultraviolet-visible (UV–VIS) detector was developed for the separation and determination of Sudan dyes (I, II, III, and IV) and Para Red in red chilli peppers. The chromatographic separation was achieved on a reverse phase C₁₈ column with isocratic elution, using a mobile phase of acetonitrile/methanol (80:20, v/v); detector was set at 506 nm. All four Sudan dyes and Para Red were separated in less than 9 min. Among 80 red chilli peppers screened, only one of them contained 0.10, 0.04, and 0.05 mg/kg Sudans I, III, and IV, respectively. No Sudan II and Para Red were detected in any of the red chilli peppers analysed. The method was ‘in-house’ validated using red chilli peppers based on following criteria: limit of detection (LOD), limit of quantification (LOQ), recovery, repeatability, reproducibility, and linearity in red chilli peppers. Depending on the dye involved, LOD and LOQ were in the range of 1.2–5.4 and 4–18 μg/kg in red chilli, respectively. The recovery, repeatability (expressed as coefficient of variation, CV_r), and reproducibility (CV_R) varied from 89 to 98%, from 0.82 to 4.09%, and from 1.33 to 4.65%, respectively. Linearity obtained for all dyes and Para Red were all r² > 0.9999 (in the range of 0.01–5 mg/l). The applicability of the method to the determination of Sudan dyes and Para Red in red chilli peppers was demonstrated. This method has potential to be used for illegal Sudan dyes and Para Red in red chilli peppers and some foodstuffs due to its simple, reliable, rapid, and excellent precision.     

Simultaneous quantitative determination of Sudan dyes using liquid chromatography–atmospheric pressure photoionization–tandem mass spectrometry

Atmospheric pressure photoionization–tandem mass spectrometry (APPI–MS/MS) method has been developed for quantitative determination of Sudan I to IV dyes. This study demonstrates the applicability of a simple isocratic normal phase HPLC method using isopropanol (0.3%) in n-hexane as the mobile phase for the separation of these dyes. A simple extraction procedure using n-hexane has been applied for the extraction of these dyes from spiked samples of chilli powder and tomato sauce. The quantitative determination of Sudan I to IV is obtained from the spiked tomato sauce and chilli powder samples by external standard method under single reaction monitoring (SRM) mode. The study includes a detailed investigation on LOD, LOQ, linearity and recovery of Sudan I to IV dyes. The LOD ranged from 5–18 μg/l and LOQ ranged from 10–24 μg/l. The present method can be a powerful analytical tool for the simultaneous quantitative determination of Sudan dyes present in food products.