Molecularly imprinted solid-phase extraction combined with high-performance liquid chromatography for analysis of trace olaquindox residues in chick feeds

BACKGROUND: Olaquindox, one of the antimicrobial growth accelerants, is usually used as a feed additive in livestock production to improve feed efficiency. Due to health concerns over possible carcinogenic, mutagenic and photoallergenic effects of olaquindox on animals, the development of a simple, rapid and sensitive analytical method for determination of olaquindox is crucial and necessary. RESULTS: In this paper, a novel and hydrophilic functionalised material of olaquindox‐imprinted polymer was synthesised in aqueous solution by a surface molecular imprinting in combination with a sol–gel process. This imprinted material was characterised by Fourier transform infrared, scanning electron microscopy, and static and kinetic adsorption experiments, and results showed that it had good recognition and selective ability, and fast adsorption‐desorption dynamics for olaquindox. Applying the prepared material as sorbent, a method of molecularly imprinted solid‐phase extraction (MISPE) for separation and analysis of olaquindox residues in feeds coupled with HPLC was presented. Under the selected MISPE condition, the detection limit (S/N = 3) for olaquindox was 68.0 ng L^?1, the RSD for five replicate extractions of 50 µg L^?1 olaquindox was 9.8%. The blank chick feed samples spiked with olaquindox at 0.0025 and 0.010 mg g^?1 levels were extracted and determined by the developed method, with recoveries ranging from 90% to 96%. CONCLUSION: This method was applied for enrichment and analysis of olaquindox in animal feed samples with good accuracy and repeatability. This study will provide a sensitive and fast method for the monitoring of olaquindox residues in foods. Copyright © 2011 Society of Chemical Industry     

在线固相萃取液相色谱-串联质谱法同时测定食品中的敌敌畏和敌百虫

目的：利用在线固相萃取超高压液相色谱-串联质谱技术建立了猪肉、火腿和腊肉中敌敌畏和敌百虫的同时检测方法。方法：样品中的目标化合物经50%乙腈水溶液提取,上清液用水稀释后经Xbridge C8柱富集,BEH C18色谱柱分离,甲醇和水梯度洗脱,三重四极杆质谱电喷雾正离子模式下采集数据,基质匹配外标曲线法定量。结果：敌敌畏和敌百虫的线性范围为0.2~50 μg/kg,相关系数r2>0.99;猪肉、火腿和腊肉中敌敌畏的定量限分别为0.2、0.2和0.5 μg/kg,敌百虫的定量限分别为0.5、0.5和1.0 μg/kg。3个加标水平的平均回收率为75.6%~104.9%,相对标准偏差<20%。结论：与已有的检测技术相比,该方法快速、简单、灵敏度高,适用于猪肉、火腿和腊肉中敌敌畏和敌百虫的同时检测,为相关食品中非法添加物的检测提供了技术支持。     

全自动分子印迹固相萃取高效液相色谱法测定食用油中10种多环芳烃

为快速测定食用油中的多环芳烃,建立全自动分子印迹固相萃取高效液相色谱法测定食用油中10种多环芳烃的分析方法。将样品用正己烷溶解,以2 mL正己烷为淋洗液,二氯甲烷为洗脱剂,经全自动分子印迹固相萃取柱净化,氮吹后定容进高效液相色谱仪(配荧光检测器)检测。结果表明：所建方法线性关系良好,检出限为0.1～1.3μg/kg,定量限为0.3～4.0μg/kg;方法的准确度良好,精密度高,10种多环芳烃在玉米油和花生油基质中的加标回收率为79.2%～114.3%,相对标准偏差为0.4%～5.7%,将该方法应用于实际食用油样品中苯并[a]芘的测定,所测样品中苯并[a]芘含量均未超出国标限量。所建方法前处理简单快速,可实现固相萃取柱的自动化处理,减少有机溶剂的消耗,适合食用油中多环芳烃的快速测定。     

固相萃取柱净化-高效液相色谱法测定谷物中的呕吐毒素残留量

目的 建立固相萃取柱净化-高效液相色谱法快速检测小麦、大麦、玉米及大米等谷物中呕吐毒素的残留量。方法 样品经乙腈-水提取液(85:15, V:V)提取,过HLB固相萃取柱净化。采用C_18柱为分离柱,对流动相的组成和洗脱斱式等参数进行优化和探讨。以水和甲醇为流动相进行梯度洗脱,流速为0.8 mL/min,柱温35℃,外标法定量。结果 呕吐毒素浓度在0.05～5.0 mg/L的范围内线性关系良好,相关系数均大于0.9999。呕吐毒素在0.5、1.0和2.0 mg/L添加水平的回收率为79.7%～106.0%,相对标准偏差(relative standard deviation,RSD)小于4.2%(n=5),斱法定量限为300μg/kg。结论 该斱法简便、快捷、准确、灵敏度较高,适用于小麦、大麦、玉米及大米等的谷物中呕吐毒素的快速检测。     

A new liquid–liquid extraction method for determination of 6 azo-dyes in chilli products by high-performance liquid chromatography

A liquid–liquid extraction method was developed for purifying and enriching the sample of 6 azo-dyes (including Para red, Sudan red G, Sudan I, Sudan II, Sudan III and Sudan IV) by formic acid and chloroform. The results indicated that formic acid can facilitate the solution of fat-soluble azo-dyes, which was helpful for the separation of the fat-soluble interferences from the samples. The extracting conditions of 6 azo-dyes were also optimised. And the proposed extraction method was evaluated by the determination of 6 azo-dyes in chilli products. The mean recoveries of 6 azo-dyes were from 94.1% to 99.2% for chilli powder and from 94.2% to 98.6% for chilli spice. The CCα and CCβ obtained for 6 azo-dyes were in the range of 1.7–2.1 and 2.8–3.4 μg/kg for chilli spice and chilli powder. The inexpensive and simple method was acceptable for routine monitoring 6 azo-dyes in chilli products.     

固相萃取-高效液相色谱法测定烟草样品中植物色素的研究

研究了固相萃取-高效液相色谱测定烟草样品中的植物色素的方法。烟草样品中的植物色素用Sep-Park-C₁₈固相萃取小柱预分离和富集,以C₁₈为固定相,(1+1)甲醇异丙醇溶液-水梯度为流动相,各组分均在最大波长下提取色谱图计算峰面积定量。方法标准回收率为92%~10 1%,RSD为1.2 4%~2.31%。用该方法研究了烤烟新鲜烟叶烘烤过程中色素变化,结果令人满意。      

分子印迹固相萃取–高效液相色谱法的优化及在测定植物油中苯并(a)芘含量的应用

建立优化的分子印迹固相萃取超高效液相色谱法测定植物油中苯并芘的检测方法。实验过程中通过对样品不同固相萃取净化效能、最佳检测波长、流动相体系及色谱柱使用的考察,结果表明,分子印迹固相萃取净化柱比较适合植物油样品的前处理萃取及净化,最佳检测波长为激发波长365 nm和发射波长410 nm,苯并芘色谱峰在此条件下具有较高的响应值和信噪比,在90%乙腈–10%水流动相体系下,目标峰具有较好的分离效果,采用150 mm的短柱子能有效提高工作效率。苯并芘在浓度0.3~20 μg/L范围内具有良好的线性关系,相关系数大于0.999 9,方法检出限为0.05 μg/kg,定量限为0.10 μg/kg,3个添加浓度水平的平均回收率为87.6%~95.9%,相对标准偏差为1.08%~2.16%。实际样品检测中,苯并芘的检出率为39.0%,超标率为2.4%,合格率为97.6%。该优化方法灵敏度高,操作便捷,快速准确,可适用于植物油中苯并芘的批量检测及污染监测情况分析。     

Molecularly imprinted solid-phase extraction coupled to liquid chromatography for determination of Sudan dyes in preserved beancurds

New molecularly imprinted microspheres synthesized by suspension polymerisation using phenylamine and naphthol as mimic template were successfully applied as selective sorbents for the solid-phase extraction used for the simultaneous determination of four Sudan dyes from preserved beancurd products. The obtained imprinted microspheres showed good recognition and selectivity to the four Sudan dyes in aqueous solution and the affinity could be easily controlled by adjusting the property of the solution. Under the selected experimental condition, the recoveries of the Sudan dyes in preserved beancurds at three spiked levels were ranged between 90.2-104.5% with the relative standard deviation of less than 6.8%. The limit of detection (LOD) and limit of quantification (LOQ) based on a signal-to-noise of 3 and 10 were in the range of 0.005-0.009 μg g⁻¹ and 0.015-0.030 μg g⁻¹, respectively. Comparing with alumina and C₁₈-based extraction, the selectivity and repeatability of molecularly imprinted solid-phase extraction (MISPE) were obviously improved. This method could be potentially applied for the determination of Sudan dyes in complicated food samples.     

分散式固相萃取结合高效液相色谱法快速测定 油脂中三种抗氧化剂含量

目的 采用分散式固相萃取技术结合高效液相色谱(HPLC),建立了食用油脂中叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、特丁基对苯二酚(TBHQ)残留的快速检测方法。方法 采用中性氧化铝作为吸附剂, 以整合了吸附剂活化、目标物提取和样品净化等步骤的“一步式”前处理方式净化样品, 最后用高效液相色谱二极管阵列检测器(DAD)对三种抗氧化剂含量进行测定。结果 在优化实验条件下, 方法的线性范围为0.2 ~200 mg/L,线性相关系数R₂≥0. 9993,对BHA、BHT、TBHQ的检出限(S/N=3)均为0.5mg/kg,回收率为85.5% ~ 95.4%,峰面积的相对标准偏差为2.10% ~ 3.53% 。结论 本文所建立的方法较液液萃取、固相萃取、凝胶渗透色谱等传统的方法更为简便快速,高效环保,成本低廉,可满足油脂中BHA、BHT、TBHQ含量检测需求;整个样品前处理过程仅需10 ~ 15分钟,适合BHA、BHT、TBHQ含量检测的批量实验。     

在线净化/固相萃取-高效液相色谱法测定柑橘中 多菌灵痕量残留量

目的 通过在线净化/固相萃取-高效液相色谱技术建立测定柑橘中痕量多菌灵的方法。方法 样品在固相萃取小柱Cyclone-MCX中进行净化和富集后,通过阀将固相萃取小柱切换至分析流路,使待测物从富集柱冲洗至分析柱PA_ⅡC₁₈中,采用梯度洗脱方式完成多菌灵的分离和检测。结果 多菌灵在1～20μg/L范围内呈线性相关,线性方程为y=0.0921x-0.0016,相关系数r=0.9995;检出限为0.1μg/L(S/N=3);柑橘中3个水平添加回收率(n=6)在81.0%～96.7%;6次加标回收相对标准偏差在2.34%～3.11%。结论 建立的此套方法简便、快速、准确、重现性好,能够满足柑橘中多菌灵痕量残留量的测定。     

固相萃取-高效液相色谱法同时测定食品中16种禁限用色素

目的建立一种高效、准确、同时测定食品中16种禁限用色素(柠檬黄、新红、苋菜红、胭脂红、日落黄、酸性品红6B、诱惑红、酸性红13、丽春红2R、丽春红SX、酸性橙I、赤藓红、酸性黄11、酸性蓝113、罗丹明B、分散红1)的方法。方法待测样品先后经0.5%氨水和乙醇+氨水+水提取、经OasisHLB固相萃取柱净化后,以Eclipse XDB C18(150 mm×4.6 mm, 5?m)为分离柱,甲醇和10 mmol/L乙酸铵为流动相进行梯度洗脱,流速为0.8 mL/min,检测波长为470、520、550和490 nm的条件下用高效液相色谱法进行测定,外标法定量。结果 16种禁限用色素在此次方法下有较好的线性关系(r≥0.9997),检出限(S/N=3)为33.0～144.0μg/L。结论本研究建立的固相萃取-高效液相色谱法可以同时测定食品中16种禁限用色素,且方法高效、准确。     

固相萃取柱高效液相色谱法检测粮食中玉米赤霉烯酮

建立固相萃取柱净化、高效液相色谱检测粮食中玉米赤霉烯酮方法。样品经乙腈—NaCl溶液(90:10,V/V)超声波提取,固相萃取柱净化,甲醇-水(70:30,V/V)为流动相,流速1 ml/min;荧光检测器检测,激发波长274 nm、发射波长440 nm;柱温30℃;进样量10μl。玉米赤霉烯酮浓度在10～600μg/L范围呈线性,线性回归方程为:Y=5.86 x+23.25,相关系数为0.9997;方法检出限为5μg/kg;3个不同水平加标平均回收率为80.4%～88.5%,相对标准偏差(RSD)为2.5%～5.4%。该法选择性高、净化效果好、操作简单、检测效果理想,适于大批量样品检测,有利于推广。     

固相萃取-高效液相色谱法检测油炸薯条中丙烯酰胺

目的 建立了一种采用固相萃取-高效液相色谱(SPE-HPLC)测定油炸薯条中丙烯酰胺的方法.方法 样品用2.0 mol/L氯化钠溶液进行提取,使用Styre Screen H2P固相萃取柱(200 mg/3 ml)净化,然后用Sapphire C18反相色谱柱进行分析,流动相为甲醇/水(5∶95),流速为1.0 ml/min,检测波长为200 nm.结果 在1.0 ～ 10.0 μg/g的添加水平范围内,样品中丙烯酰胺的平均回收率为66.2％ ～80.9％,相对标准偏差为1.6％ ～2.1％,最低检测限和最低定量限分别为0.025和0.080 μg/g.结论 该方法操作简单、快速、准确,可用于油炸薯条中丙烯酰胺的快速测定.     

基于固相萃取-高效液相色谱法的纺织品中三氯生的测定

建立了纺织品中三氯生的固相萃取-高效液相色谱检测方法。样品经超声提取后,用固相萃取进行净化,Kromasil C18 柱（250 mm × 4.6 mm i.d., 5 μm）分离,采用水/乙腈 (15/85, V/V)为流动相,紫外检测波长为280 nm,外标法定量。实验结果显示：样品中的三氯生在0.1~20.0 mg/kg的浓度范围内呈良好的线性关系,最低检出限LOD为0.01mg/kg,定量检出限LOQ为0.05 mg/kg 。方法回收率在94.0%~100.4%之间,RSD 为2.0%~4.4% 。本方法简便、快速、专属性强、干扰少,能满足纺织品中三氯生的测定要求。     

分散固相萃取-高效液相色谱法测定饮料和糖果中3种人工合成色素

以聚苯乙烯-聚4-乙烯基吡啶(PS@P4VP)复合微球为固相萃取材料,用于柠檬黄、赤藓红和日落黄3种人工合成色素的分析检测,探究了该微球的吸附性能与最佳固相萃取条件,建立了芬达(橙味)汽水和水果糖中3中色素的分散固相萃取-高效液相色谱(DSPE-HPLC)检测方法。结果表明,PS@P4VP对3种色素有较好的吸附性能,且可多次重复使用。柠檬黄和日落黄的最佳吸附pH为3.0,吸附平衡时间分别为20、90 min;赤藓红的最佳吸附pH为5.0,吸附平衡时间为60 min。PS@P4VP 对柠檬黄、赤藓红和日落黄的吸附过程均符合准二级动力学模型和Langmuir等温吸附模型,最大吸附容量分别为47.17、32.47、43.67 mg/g。结合实际样品分析结果表明,以PS@P4PV为固相萃取材料的高效液相色谱检测方法在芬达(橙味)汽水和水果糖中对3中色素有较好的分离检测效果,加标回收率为92.03~105.51%。     

固相萃取-高效液相色谱-串联质谱法同时测定鸡蛋中42种农药残留

目的 建立固相萃取-高效液相色谱-串联质谱法同时测定鸡蛋中42种农药残留的检测方法。方法 样品经加水分散后,用乙腈提取,PRiME HLB固相萃取柱进行净化处理,采用Shim-pack XR-ODSⅡ色谱柱(75 mm×2.0 mm, 2.2 μm)分离,5 mmol乙酸铵水溶液(A)-甲醇溶液(B)为流动相,进行梯度洗脱;质谱法选择电喷雾离子源ESI,正负离子分段扫描,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。结果 42种农药的峰面积与质量浓度在0.1~2 ng/mL范围内呈现良好的线性关系,相关系数r均大于0.994;方法检出限(LOD, S/N=3)为0.04~0.3 μg/kg,定量限(LOQ, S/N=10)为0.1~1.0 μg/kg。在1.0、2.0、5.0、10 μg/kg四个添加水平下,42种农药平均加标回收率为61.0%~118.5%,相对标准偏差为0.8%~9.9%。结论 该方法具有操作简单、分析时间短、试剂用量少、灵敏度高且重复性好等特点,适用于鸡蛋中农药残留的高通量快速检测分析。     

A rapid shaking-based ionic liquid dispersive liquid phase microextraction for the simultaneous determination of six synthetic food colourants in soft drinks,sugar- and gelatin-based confectionery by high-performance liquid chromatography

A novel and simple rapid shaking-based method of ionic liquid dispersive liquid phase microextraction for the determination of six synthetic food colourants (Tartrazine, Amaranth, Sunset Yellow, Allura Red, Ponceau 4R, and Erythrosine) in soft drinks, sugar- and gelatin-based confectionery was established. High-performance liquid chromatography coupled with an ultraviolet detector was used for the determinations. The extraction procedure did not require a dispersive solvent, heat, ultrasonication, or additional chemical reagents. 1-Octyl-3-methylimidazolium tetrafluoroborate ([C₈MIM][BF₄]) was dispersed in an aqueous sample solution as fine droplets by manual shaking, enabling the easier migration of analytes into the ionic liquid phase. Factors such as the [C₈MIM][BF₄] volume, sample pH, extraction time, and centrifugation time were investigated. Under the optimum experimental conditions, the proposed method showed excellent detection sensitivity with limits of detection (signal-to-noise ratio = 3) within 0.015–0.32 ng/mL. The method was also successfully used in analysing real food samples. Good spiked recoveries from 95.8%–104.5% were obtained.     

固相萃取—超高效液相色谱法测定水产品中6种氟喹诺酮类药物残留

基于固相萃取(SPE)和超高效液相色谱(UPLC)技术,建立可同时测定水产品中诺氟沙星、氧氟沙星、环丙沙星、培氟沙星、洛美沙星、恩诺沙星6种氟喹诺酮类药物残留量的检测方法。经优化后的检测过程及参数为:样品匀浆后以磷酸盐缓冲液为提取剂,提取液经SPE净化、氮吹浓缩后,残渣用0.2%的甲酸水溶液溶解供UPLC分析;选用BEH C18(1.7μm,2.1mm×50 mm)色谱柱,以体积比为937的0.05mol/L柠檬酸+0.1 mol/L乙酸铵缓冲液-乙腈为流动相,流速为0.42mL/min,进样体积为0.2μL,柱温为50℃,荧光检测器检测波长λex=278nm、λem=465nm。该方法简单有效,添加回收率为63.69%～90.83%,最低检出限为0.5～1.8μg/kg,相对标准偏差均低于10%。