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.     

二维液相色谱法测定烧烤肉制品中苯并（a）芘

烧烤肉制品由于富含动物油脂,在炭火高温烧烤熟制品过程中,容易出现苯并（a）芘超标问题,具有较高安全隐患。建立二维液相色谱仪检测烧烤肉制品中苯并（a）芘的方法。第1维为分离、富集柱,采用Inertsil ODS柱（4.6 mm×150 mm,5 μm）,流动相为乙腈-水（85∶15,V/V）,流速1.0 mL/min,可以实现500 μL样品中目标物苯并（a）芘的富集与分离;第2维采用ChromSpher Pi柱（3.0 mm×80 mm,5 μm）,流动相为异丙醇-乙腈（60∶40,V/V）,流速1.2 mL/min,可以有效分离、测定样品中的苯并（a）芘。结果表明：烧烤肉制品中苯并（a）芘在1.0～20.0 ng/mL范围内呈线性关系,其线性回归方程为y=1.847 1x－0.103 3（r=0.999）,检出限为0.08 μg/kg,在1.00、3.00、5.00、10.00 μg/kg加标水平下,加标回收率为97.1%～105.2%,相对标准偏差为1.55%～2.77%。     

二甲亚砜提取—冷冻离心净化测定食品中苯并[a]芘及苯并[e]芘

建立以二甲基亚砜作为提取溶剂,冷冻离心提取净化食品中的苯并[a]芘和苯并[e]芘,高效液相色谱—荧光法检测的方法。替代传统的固相萃取小柱净化方式,能更快速、高效、准确检测食品中苯并[a]芘和苯并[e]芘的含量。2种目标物在0.5~1 000 ng/mL范围内呈现良好线性关系,在1~100 ng/g添加量下,回收率为89.0%~91.3%,相对标准偏差为1.19%~1.29%;仪器检出限为0.01 ng/mL,植物油脂方法检出限为0.05 ng/g,肉制品和动物油脂方法检出限为0.02 ng/g。该方法测定动植物油脂和肉制品中的苯并[a]芘和苯并[e]芘方便、快捷,适用于批量化检测。     

固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘

采用中性氧化铝小柱净化样品,建立固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘的方法。样品以正己烷为提取剂,净化、蒸发浓缩后正己烷溶解,荧光检测器检测。流动相为乙腈-水(75:25,V/V),流速0.5mL/min,外标法定量。苯并(a)芘在0.10～50.0μg/L质量浓度范围内线性关系良好,相关系数R2为0.9998;在空白样品中添加3个水平的标准品,回收率在91.7%～97.5%之间,相对标准偏差均小于2%(n＝3);最低检出限为0.01μg/kg,定量限为0.03μg/kg。方法操作简便、分析时间短、稳定性好、选择性好、灵敏度高,为植物油中苯并(a)芘的测定提供参考。     

食用油中苯并（a）芘检测的样品前处理方法——相转移催化皂化法

建立了食用油中苯并（a）芘的相转移催化皂化提取前处理方法,并结合高效液相色谱（HPLC-FLD）进行含量检测。结果表明：该方法检出限为0.2 ng/mL,定量限为0.7 ng/mL,苯并（a）芘平均回收率为96.15%~103.2%,相对标准偏差为2.61%~4.96%。该方法具有降低有机溶剂的消耗、降低检测成本、操作简单、检测时间短等优点,符合快速、便捷、准确及灵敏地检测食用油中苯并（a）芘要求。     

在线净化-液相色谱法快速测定熏烤水产品中的苯并（a）芘

建立在线净化-液相色法测定熏烤水产品中的苯并(a)芘的条件及方法。使用乙酸乙酯提取后即可直接上样分析,经C8在线净化柱净化后,C18色谱柱分离,荧光检测器检测。苯并(a)芘[benzo(a)pyrene,BaP]的方法检出限为0.035 ng/mL。利用该方法对熏烤水产品中BaP进行测定,线性相关系数为0.9999,平均回收率为89.6%~99.0%,相对标准偏差为1.3%~3.1%。     

全自动固相萃取净化-高效液相色谱法测定食用植物油中苯并(a)芘含量

为提高工作效率,降低误差,建立分子印迹柱全自动固相萃取净化-高效液相色谱法测定食用植物油中苯并(a)芘含量的方法。样品经正己烷提取,采用全自动固相萃取仪进行分子印迹柱净化,C18色谱柱分离,高效液相色谱-荧光检测器检测。结果表明：苯并(a)芘在0.5～20.0 ng/mL质量浓度范围内与峰面积线性关系良好,相关系数为0.999 9,方法检出限为0.09μg/kg,定量限为0.30μg/kg,加标回收率为91.7%～111.8%,相对标准偏差为2.0%～8.2%,与国标方法的检测结果不存在显著性差异;对市售38份食用植物油样品进行检测发现,苯并(a)芘的检出率为76.3%。该方法准确度高、重复性好,可批量自动化前处理样品,提高工作效率,并降低人员操作误差风险,适用于食用植物油中苯并(a)芘含量的测定。     

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。     

金属有机骨架基质固相分散高效液相色谱法检测食用油中苯并[a]芘

目的建立基于金属有机骨架材料(metal-organic frameworks, MOFs) MIL-101(Cr)的基质固相分散进行食用油样品前处理,并以高效液相色谱串联荧光检测器(high performance liquid chromatography-fluorescence detector, HPLC-FLD)对苯并[a]芘进行定量检测。方法吸附后将体系装填于6 mL固相萃取空柱,以丙酮洗脱,氮气吹干定容。色谱流动相为乙腈-水(80:20, V:V),流速0.3 mL/min,激发波长369 nm,发射波长404 nm,外标法定量。结果苯并[a]芘在1～50ng/g范围内呈良好线性,相关系数r~2为0.9997,加标回收率为96.0%～99.9%。方法检测限及定量限分别为0.33ng/g和1.09ng/g,实际样品检测的相对标准偏差为2.8%～8.9%。结论该方法操作简单,测定结果准确,同时克服了常规固相萃取法易堵塞、渗漏、过载及负压过高等问题,可用于食用油中苯并[a]芘的检测。     

高效液相色谱法快速测定食用植物油中苯并（a）芘的研究

本文研究了食用植物油中苯并(a)芘的高效液相色谱检测法。用乙腈作为样品中苯并(a)芘的提取液,采用高效液相色谱-荧光检测器测定,外标峰面积法定量。结果表明,苯并(a)芘在0.5-20 ng/mL范围内呈良好的线性关系,相关系数为0.999 7。在空白样品中添加0.2μg/kg、5.0μg/kg、10.0μg/kg三个水平苯并(a)芘的回收率为95.8-101.3%,相对标准偏差(RSD)为1.72-10.13%,检出限为0.2μg/kg。本方法适用于食用植物油中苯并(a)芘的检测。     

Evaluation of polycyclic aromatic hydrocarbon contents and risk assessment for fish and meat products in Korea

Contents and human exposure to polycyclic aromatic hydrocarbons (PAHs) in fish and meat products in Korea were analyzed. Liquid-liquid extraction and HPLC with fluorescence detection were used. The average concentrations of total PAHs were 0.21 μg/kg for fish and shellfish, 1.97 μg/kg for meat, and 0.32 μg/kg for smoked products. The benzo[a]pyrene (BaP) content was <5 μg/kg and contents of 4 PAHs (benzo[a]anthracene, chrysene, benzo[b]fluoranthene, and BaP) were lower than 30 μg/kg, which is the maximum tolerable limit. PAHs values were changed to BaP to conduct exposure assessments and risk characterization. Dietary exposure was 0.011-0.544 ng-TEQ_BaP/kg/day. The margin of exposure for all population groups assessed at the mean and 95^th percentile was 13,757–9,090,909, of low concern. PAHs were detected in fish and shellfish, meat, and smoked products, but their contribution to human PAH exposure was small.     

Polycyclic aromatic hydrocarbons (PAHs) in meat products and estimated PAH intake by children and the general population in Estonia

The concentrations of benzo[a]pyrene and 11 other polycyclic aromatic hydrocarbons (PAHs) were analysed from 322 commercial, cured meat products and 14 home-grilled meat samples as part of the Estonian food safety monitoring programme during 2001-2005. The maximum acceptable concentration of 5 µg kg^-1 for benzo[a]pyrene was exceeded in 3.4% of samples. The highest PAH concentrations were detected in home-grilled pork samples. Using of disposable grilling unit resulted in 1.6 times higher PAH concentrations compared to the traditional wood-burning grill. The average intake of benzo[a]pyrene and sum of 12 PAHs from meat products was estimated for children (age 1-16 years) on the basis of an individual food consumption questionnaire and, for the general population, based on national food consumption data. The highest total PAH concentrations detected were 16 µg kg^-1 in smoked meat and ham, 19 µg kg^-1 in smoked sausage and 6.5 µg kg^-1 in smoked chicken samples. Since smoking and grilling are prevalent meat-cooking methods in Estonia, the impact of meat products is assessed to be significant in overall PAH intake.     

江苏地区熏烧烤肉制品质量分析

目的了解熏烧烤肉制品质量状况。方法对江苏省13市418批次熏烧烤肉制品进行抽检,采用最新食品安全国家标准进行检测,并对检测数据进行分析。结果苯甲酸及其钠盐2批次不合格,苯并[a]芘1批次不合格,4种多环芳烃之和[苯并[a]芘、苯并[a]蒽、苯并[b]荧蒽以及1,2-苯并菲总量,简写为PAH4]项目有3批次超过欧盟限量;360批次样品检出多环芳烃,检出率86.1%,分子量相对较低的轻质多环芳烃平均检出率是重质多环芳烃平均检出率的3.2倍;229批次肉制品进行了肉源性成分鉴定,发现21批次与声称成分不符,不符合率为9.2%。结论本次熏烧烤肉制品主要不合格项目为超范围使用食品添加剂、苯并[a]芘超标,PAH4超过欧盟限量标准;由肉种成分分析结果可以看出,存在以低价原料冒充高价原料的情况。     

Analysis of benzo[a]pyrene content from smoked food products in Korea

The content of benzo[a]pyrene (BaP) was evaluated from 100 smoked food products commonly consumed in Korean market with HPLC. Analysis method for BaP content on smoked food products was evaluated and validated. For validation, the efficiency of saponification time and solid phase extraction cartridges were evaluated. During 1–4 h of saponification, recovery of BaP was ranged from 90.17 to 98.87%. Among the 5 tested cartridges including florisil, silica gel, and alumina cartridges (acidic, basic, and neutral), the most efficient cartridge was florisil cartridge and the recovery of BaP was 98.87%. Limit of detection and limit of quantification was 0.03 and 0.09, respectively. As a result of BaP content analysis from smoked food products, the average BaP content was 0.45 μg/kg and the highest content of BaP was 2.87 μg/kg detected in smoked salmon product.     

Polycyclic aromatic hydrocarbons in food samples collected in Barcelona, Spain

This study reports on the concentrations of eight polycyclic aromatic hydrocarbons (PAHs) in food samples collected in the city of Barcelona (Catalonia, Spain) from 2003 to 2004. Food samples included meat products, fish (fresh and smoked), other seafood (cephalopods, crustaceans, and bivalves), vegetable oil, and tea. Concentrations of benz[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[g,h,i]perylene, benzo[alpha]pyrene, benzo[e]pyrene, dibenz[a,h]anthracene, and indeno[1,2,3-c,d]pyrene were determined by reversed-phase high-performance liquid chromatography with fluorescence detection. PAHs were detected in most tea samples (94%), which had the highest concentration of total PAHs (mean concentration of 59 microg/kg). Other food groups with a high presence of PAHs were bivalves (present in 34% of the samples; mean value of 2.7 microg/kg) and meat products (present in 13% of the samples; mean value of 1.7 microg/kg). The PAHs detected most frequently were benzo[e]pyrene and benzo[b]fluoranthene. No sample had levels above current regulation standards. Nevertheless, the frequent presence of PAHs in bivalves, tea samples, and meat products, together with the fact that dietary sources are the main exposure to these carcinogenic compounds, suggests the need for some monitoring scheme to follow up on these trends.     

烟熏工艺对清真牛肉香肠品质的影响

以烟熏清真牛肉香肠为研究对象,研究木熏工艺和液熏工艺对产品品质的影响,以期为烟熏液生产和液 熏工艺的改进提供技术支持。从感官评价、色泽、苯并（a）芘、挥发性风味成分和货架期5 个方面进行对比, 比较两种烟熏工艺对清真牛肉香肠品质的影响。结果表明,传统的木熏工艺的产品在风味方面具有明显的优势, 木熏工艺产品中酚类物质的相对含量达到16.95%,液熏工艺产品中仅为11.58%;而液熏工艺的产品在苯并（a） 芘含量方面具有明显的优势,烟熏40 min的产品中苯并（a）芘的含量为2.84 μg/kg,而液熏4 次的产品中苯并 （a）芘的含量仅有0.95 μg/kg;在色泽和货架期方面并没有明显的差异。因此,需要进一步重点提高烟熏液的风 味成分,使其更接近传统木熏工艺的产品,改善烟熏清真牛肉香肠的品质,从而提高烟熏液产品的市场占有率。     

正相高效液相色谱法测定腌腊肉制品中磷脂酰胆碱氢过氧化物的含量

采用正相高效液相色谱法对腌腊肉制品中的磷脂酰胆碱氢过氧化物（PC-OOH）进行检测。腌腊肉制品中的PC-OOH用氯仿-甲醇（2∶1,V/V）提取,以合成的C16∶0/18∶2 PC-OOH为标样,采用正相高效液相色谱-紫外法进行检测。色谱柱：Lichrosorb Si60（250 mm×4.0 mm,5 μm）;流动相：A为水,B为正己烷-异丙醇（3∶2,V/V）,采用梯度洗脱;流速：1 mL/min;柱温：30 ℃;检测波长：234 nm。结果表明：C16∶0/18∶2 PC-OOH在20～600 nmol/mL范围内呈现良好的线性关系（R2=0.999 9）,检出限为5.8 nmol/mL,定量限为19.4 nmol/mL,不同水平的平均回收率为79.4%～91.9%。实际样品分析显示,农家腊肠A、B和火腿中方样品中PC-OOH的含量比较高,为92.4、106.4 nmol/g和102.5 nmol/g,烟熏肉中未检出PC-OOH。本实验建立的分析方法简便快捷、具有较好的灵敏度和可靠性,可用于腌腊肉制品中PC-OOH的定量分析。