固相萃取-HPLC法同时测定肉制品中苋菜红、胭脂红、日落黄和诱惑红含量

建立了利用固相萃取-高效液相色谱法同时测定肉制品中4种合成色素的检测方法。样品经乙醇+氨水+水(7+2+1,v/v/v)提取后,固相萃取净化,经C18柱分离,用紫外检测器检测。4种合成色素分离良好,加标平均回收率为66.7%~99.7%,相对标准偏差1.9%~3.6%。该方法准确度和精密度较高,可应用于测定肉制品中的合成色素,结果令人满意。     

全自动固相萃取-液相色谱法测定肉制品中的合成色素

建立了一种快速、高效、准确的测定肉制品中柠檬黄、苋菜红、胭脂红、日落黄、诱惑红5种合成色素的全自动固相萃取-高效液相色谱(SPE-RP-HPLC)方法。方法:样品采用固相萃取小柱进行净化、富集,在C18柱色谱柱上以甲醇-乙酸铵水溶液(20.0mmol/L)为流动相实现基线分离,紫外检测。结果:5种合成色素的加标回收率为88.4%~96.0%,精密度为1.8%~3.1%。结论:本法可用于肉制品中柠檬黄、苋菜红、胭脂红、日落黄、诱惑红5种合成色素的测定。     

固相萃取-高效液相色谱法测定肉制品中苯并(a)芘

建立固相萃取-高效液相色谱法测定肉制品中苯并(a)芘的检测方法.样品经Cleanert BaP固相萃取柱净化、浓缩,Waters SunFire C18(4.6mm×250mm,5μm)色谱柱进行分离,流动相为乙腈-水(88∶12,V/V),流速1.0mL/min,荧光检测器,激发波长386nm,发射波长405nm.结果表明,苯并(a)芘在线性范围0.5～10ng/mL内,相关系数为0.9978,最低检出限为0.04μ g/kg,精密度(RSD)小于5％,回收率82.2％～94.9％.本方法快速简便、重现性好,可以用于肉制品中苯并(a)芘含量的测定,为肉制品的质量控制和安全评价提供保证.     

阴离子固相萃取-HPLC法测定肉制品中13种合成色素

建立阴离子固相萃取-高效液相色谱（high performance liquid chromatography,HPLC）法同时测定肉制品中13种易于滥用的合成色素的检测方法。样品经石油醚除去脂肪后,以氨水乙醇溶液提取,结合低温冷冻法除去蛋白质,通过阴离子固相小柱批量富集净化后,用2%（体积分数）氨水甲醇洗脱,洗脱液氮吹浓缩后得供试液,采用Waters XBridge Shield RP18（250 mm×4.6 mm,5 μm）色谱柱分离,以甲醇和0.02 mol/L乙酸铵为流动相进行梯度洗脱,经二极管阵列检测器分析,外标法定量。13种目标化合物在0.1 μg/mL～10.0 μg/mL质量浓度范围内线性良好,相关系数r均高于0.999 5;检出限为0.2 mg/kg～0.5 mg/kg,定量限为0.6 mg/kg～1.5 mg/kg;平均加标回收率为65.2%～102.0%;精密度（n=6）在6.0%以内。采用该方法检测156批肉制品,12批肉制品中检出目标色素,含量范围在0.23 mg/kg～15.7 mg/kg之间,检出色素包括常见的酸性红、苋菜红及日落黄,还发现有非法添加红2G和酸性橙Ⅱ。该方法适用于含有大量脂肪和蛋白质的肉制品中多种合成色素的同时测定。     

固相萃取-高效液相色谱法同时测定蔬菜制品中11种合成着色剂

建立一种固相萃取-高效液相色谱法同时测定蔬菜制品中11种人工合成着色剂的方法。蔬菜制品中的合成着色剂经25%的氨水乙醇提取,弱阴离子固相萃取小柱Waters Oasis WAX净化,Agilent 5 TC-C18(2)为分离柱,甲醇∶乙腈(4∶1,体积比)-0.02 mol/L乙酸铵溶液为流动相进行梯度洗脱,用二极管阵列检测器多波长检测,外标法定量。结果显示,11种色素在0.2μg/mL～40μg/mL范围内具有良好的线性,在1、2、10 mg/kg 3个加标水平下的平均回收率为87.5%～102.6%,相对标准偏差为1.5%～5.8%,检出限在5μg/L～45μg/L。该方法可用于蔬菜制品中人工合成着色剂的日常检测。     

固相萃取-高效液相色谱法同时测定海米中10 种合成色素

建立固相萃取-高效液相色谱法同时测定海米中新红、柠檬黄、日落黄、胭脂红、偶氮玉红、苋菜红、诱惑红、亮蓝、赤藓红、罗丹明B 10 种合成色素的方法。海米中的合成色素用氨化乙醇提取、固相萃取柱净化,ODS-3 C18柱为分离柱,甲醇和0.02 mol/L乙酸铵为流动相梯度洗脱,采用二极管阵列检测器,在360 nm波长处检测,外标法定量。10 种合成色素在0.2～50 mg/L质量浓度范围内与其峰面积成良好的线性关系;10 种合成色素的检出限为0.4～1.0 mg/kg。3 个不同加标水平的回收率为74.3%～90.0%,相对标准偏差小于4.3%。该方法能同时完成10 种合成色素的测定,可用于海米中合成色素的检测分析。     

分散固相萃取-超低温液液微萃取-气相色谱质谱法测定烟熏及烧烤肉制品中16种欧盟优控多环芳烃

建立了分散固相萃取-超低温液液微萃取-气相色谱质谱法测定烟熏及烧烤肉制品中16种欧盟优控多环芳烃的分析方法.样品用乙腈提取、上清液经分散固相萃取净化后在-80℃条件下采用甲苯液液微萃取浓缩,选用DB-EUPAH色谱柱(20 m×0.18 mm×0.14μm)分离,最后经质谱检测定量.结果表明,16种欧盟多环芳烃在5～5...     

固相萃取-HPLC法检测熟肉制品中合成色素

建立固相萃取-高效液相色谱法同时测定熟肉制品中柠檬黄、苋菜红、胭脂红、日落黄4种合成色素的方法。熟肉制品绞碎后加入乙醇+氨水(75+25)溶液,经涡旋分散、超声提取,固相萃取柱净化后,采用一台液相仪器、两根Kromasil C18柱串联分离,以甲醇和5 mmol/L乙酸铵水溶液为流动相进行洗脱,用二极管阵列检测检测器在254 nm波长下检测。该方法在10 ng~160 ng范围内线性关系良好(r≥0.999 8);4种色素回收率为87.0%~95.5%,检出限为0.04 mg/kg~0.05 mg/kg,相对标准偏差为2.37%~6.76%。该方法能同时分析熟肉制品中4种合成色素,并能得到稳定准确的结果,节约检测时间。     

液相色谱串联质谱测定动物源性食品中孕激素类药物残留

本文以常见的肉制品为研究对象,建立并优化了经过固相萃取小柱净化,结合LC-MS/MS测定肉制品中8种孕激素残留量的方法.样品经过酶解提取,之后经C18小柱净化后,采用液相色谱串联质谱对孕激素进行检测分析.结果表明,8种孕激素分离效果好,检出限(LOD)为0.01-0.05 μg/kg,相对标准偏差＜4.0％(n = 6...     

固相萃取-高效液相色谱法测定自制饮料中10种合成色素的含量

建立一种固相萃取-高效液相色谱法测定自制饮料中10种常见合成色素含量的方法。样品经25%氨化甲醇提取,冷冻沉淀法除蛋白后,采用固相萃取柱净化富集,以Agilent5HC-C18(2)(4.6mm×250mm,5μm)为色谱柱进行分离,甲醇和0.02mol/L乙酸铵为流动相进行梯度洗脱,二极管阵列检测器[扫描范围(190～700)nm],选择254 nm作为检测波长,外标法定量分析。结果表明,10种常见合成色素的线性关系良好,线性范围为(0.1～5.0)mg/L,相关系数为0.9996～0.9999;检出限为(0.012～0.024)mg/L,平均回收率为91.2%～101.4%(n=3),相对标准偏差为0.6%～2.4%。该方法操作简单、快速、结果准确性高,可广泛用于自制饮料中10种常见合成色素的含量测定。     

索氏提取-固相萃取-高效液相色谱法检测烟熏肉制品中苯并(a)芘

采用索氏提取-固相萃取-高效液相色谱法检测清真牛肉香肠中的苯并(a)芘含量,结果表明,该方法操作简单,检测结果准确,可信度高,回收率可以达到91%以上,特别是对于油脂含量较高的食品具有良好的效果,可以推广到其他肉制品中苯并(a)芘的检测。     

高效液相色谱法测定肉制品中栀子黄色素含量

通过正交试验分析法对肉制品中栀子黄色素提取方法进行优化。利用正交试验设计考察提取溶剂体积、超声时间和提取次数对肉制品中栀子黄色素提取回收率的影响。结果表明,肉制品中栀子黄色素的最优提取条件为：甲醇为提取溶剂、固液比1∶6（g/mL）、超声提取时间20 min、提取2 次;建立高效液相色谱法测定肉制品中栀子黄色素中藏花素和藏花酸方法的线性范围为0.5～50 mg/mL,相关系数大于0.999,检出限不高于0.07 μg/g,加标平均回收率为83.51%～96.00%,相对标准偏差不大于2.94%。该方法准确度高、简单、快速,可适用于肉制品中栀子黄色素中藏花素和藏花酸含量检测。     

Modification of the ion exchange HPLC procedure for the detection of nitrate and nitrite in dairy products

Existing ion exchange HPLC methodology for nitrate and nitrite analysis in cured meat products suffers from high analyte variability at low concentrations and also chromatographic interference by artifacts in some other foods, such as dairy products. An investigation into the sources of variability has shown that both the cyclohexyl solid phase extraction cartridge and the glass fibre filter used in the original method can introduce artifacts which interfere with the determination of the nitrate in foodstuffs. We have also found that the use of a graphitized solid phase extraction cartridge used in tandem with the cyclohexyl solid phase extraction cartridge removed the artifacts from the chromatograph of dairy products that co-eluted with nitrite and nitrate. Values for the nitrite and nitrate content of dairy products were obtained by the HPLC procedure using these two solid phase extraction cartridges and the values obtained were in close agreement with those obtained by cadmium column reduction and colorimetry.     

固相萃取-高效液相色谱法测定食品基质中5种不同合成红色着色剂

目的建立一种固相萃取-高效液相色谱法(solidphaseextraction-highperformanceliquid chromatography,SPE-HPLC)测定食品中5种人工合成红色着色剂(新红、苋菜红、胭脂红、诱惑红、赤藓红)的方法。方法比较ProElut PWA-2, Cleanert PWAX和Sep-Pak Plus QMA 3种不同SPE小柱的净化效果,比较Eclipse XDB C_(18)、Venusil XBP C_(18)及Agilent TC-C_(18) 3种色谱柱对5种着色剂的分离情况,按照GB 5009.35-2016《食品中合成着色剂的测定》对食品中5种着色剂进行测定。结果 Pro Elut PWA-2 SPE固相萃取小柱进行样品净化效果最优, Agilent TC-C_(18)色谱柱在10 min内有较好的分离度。加标浓度为0.5～50 mg/kg时,该方法回收率为90.3%～103.9%,相对标准偏差(relative standard deviation, RSD)值为1.18%～7.11%。结论该方法快速、准确,适合用于不同食品基质中5种合成着色剂定性、定量测定。     

The determination of niacin in selected foods by capillary electrophoresis and high performance liquid chromatography: acid extraction

A robust method for the determination of niacin in raw and cooked meat and fish samples using acid extraction to liberate the niacin from the food matrix and capillary electrophoresis (CE) and high performance liquid chromatography (HPLC) as the determinative steps is described. Niacin is liberated from the food matrix by autoclaving in the presence of 0.8 M sulphuric acid at 121°C for 2 h. C18 and cation exchange solid phase extraction (SPE) cartridges were used to isolate and concentrate the niacin before analysis. CE analyses were performed with an uncoated 50 μm extended light path fused silica capillary column and a buffer comprising of 7.5% acetonitrile and 92.5% of a 1:1 mixture of 0.02 M potassium dihydrogen orthophosphate and 0.02 M disodium hydrogen orthophosphate pH 7. Saccharin was used as the internal standard. The levels of niacin determined by CE compared favourably with those determined by HPLC (canned ham CE 3.5 mg/100 g, HPLC 3.3 mg/100 g; raw lamb CE 7.7 mg/100 g, HPLC 7.7 mg/100 g). The average recovery of niacin added to the samples prior to extraction was 103%. The limit of reporting for the determination is 0.5 mg/100 g. The procedure was suitable for only a limited number of other food types (e.g. fruit, vegetables and nuts). Alkali extraction of these foods using saturated calcium hydroxide followed by SPE cleanup and CE determination provided more reliable results. The limit of reporting for this procedure was 0.2 mg/100 g for fruit and 0.5 mg/100 g for vegetables.     

全自动固相萃取-高效液相色谱法测定熏烤肉制品中苯并(a)芘含量

建立全自动固相萃取-高效液相色谱法检测熏烤肉制品中苯并(a)芘的方法。样品经正己烷提取、分子印迹小柱净化,高效液相色谱-荧光检测器检测,流动相为乙腈-水（90∶10,V/V）,流速1.0 mL/min。结果表明：苯并(a)芘在0.0～45.2 ng/mL质量浓度范围内线性关系良好,相关系数（R2）为0.999 7,检出限为0.12 μg/kg,回收率为97.2%～100.2%,相对标准偏差为1.4%～2.6%。该方法灵敏度高,稳定性好,批处理速度快,接触有机试剂较少,适用于熏烤肉制品中苯并(a)芘残留量测定。     

食品中红2G、二甲基黄、二乙基黄工业染料的同时测定

建立了肉制品、豆制品、调味品中红2G、二甲基黄和二乙基黄的高效液相色谱及液相色谱—质谱联用测定方法。结果表明,红2G的检出限为0.5mg/kg,二甲基黄、二乙基黄的检出限均为0.1 mg/kg,回收率为80.7%~91.8%,相对标准偏差为3.8%~7.8%。     

Automated Magnetic Solid-Phase Extraction for Synthetic Food Colorant Determination

A new automated magnetic solid-phase extraction (MSPE) method was developed and combined with high-performance liquid chromatography (HPLC) and spectrophotometry for off-line and on-line quantitative enrichment and determination of synthetic food colorants in food samples. Fe₃O₄-poly (ionic liquid) core-shell microspheres were prepared as a sorbent to quickly extract analytes from aqueous samples. The entire MSPE process, including extraction, separation, elution, and cleaning, was automated using common equipment. The main parameters affecting the performance of MSPE and the automated process, such as absorbent, sample pH, eluent, flow rate, elution time, etc., were investigated in detail. Under the optimum experimental conditions, the limits of detection ranged between 4.1 and 14 ng/mL by off-line HPLC and were 220 ng/mL for the determination of amaranth by on-line spectrophotometry, with excellent reproducibility (intra- and inter-day relative standard deviations were less than 3.2 %). The developed method was successfully applied to the determination of colorants in food samples.     

Development of Multiresidue Analysis for 21 Synthetic Colorants in Meat by Microwave-Assisted Extraction–Solid-Phase Extraction–Reversed-Phase Ultrahigh Performance Liquid Chromatography

A novel ultrahigh performance liquid chromatographic method is developed for analysis of 21 synthetic colorants with different acid–base property, solubility, and polarity. The meat samples were extracted by microwave-assisted extraction followed by cleanup with solid-phase extraction. The effective separation of the colorants in meat matrixes was achieved, and no interfering peaks could be detected at the retention time of the analytes. The calibration curves showed good linearity with correlation coefficients of 0.9940–0.9999. The limits of quantification were 0.48–7.19 μg/kg. The average recovery of the 21 analytes from meat samples spiked with 25 and 75 μg?kg^?1 was 61.29–116.1 % with relative standard deviation (RSD) of <11 %. For blank beef sausage spiked with 50 μg?kg^?1 for each analyte, the intraday precision (as RSD) for 21 analytes was 1.45–9.21 % for six determinations within a day. This method has the advantages of being rapid, sensitive, accurate, and with high-throughput and can be applied for multiresidue analysis of meat samples, including six allowable azo food colorants, ten banned azo food colorants, four banned triphenylmethanes, and rhodamin B food colorant.     

HPLC法检测蜜饯中20种合成着色剂含量

建立蜜饯中柠檬黄、新红、苋菜红、靛蓝、丽春红S、胭脂红、喹啉黄、日落黄、诱惑红、亮蓝、酸性红44、酸性红、食品红1、橙黄1、酸性红50、专利蓝V、赤藓红、酸性橙2、酸性橙8、亮蓝G共20种合成着色剂的高效液相色谱测定方法。试样用甲醇/氨水溶液提取,混合型弱阴离子反相固相萃取柱净化,甲醇/20 mmol/L乙酸铵为流动相梯度洗脱,二极管阵列检测器多波长检测,外标法定量。结果表明,该方法在0.1~20 μg/mL的线性范围内相关系数均大于0.999,加标回收率范围为84.0%~104.5%,相对标准偏差（RSD）为1.3%~5.3%。该方法操作便捷、稳定性好、回收率高,适用于蜜饯中20种合成着色剂的同时分析检测。该方法可以扩展应用于其他同结构性质的色素分析,对其他食品类别中色素的检测也具有参考意义。