QuEChERS-超高效液相色谱-串联质谱法快速测定动物源性食品中矮壮素残留

建立了QuEChERS-超高效液相色谱-串联质谱法快速测定动物源性食品中矮壮素残留的分析方法。样品经乙腈提取,无水硫酸镁、C₁₈及N-丙基乙二胺吸附剂净化,采用Venusil MP C₁₈（2）色谱柱分离,内标法定量。结果表明,矮壮素在0.05～200μg/L线性良好,相关系数（R²）为0.999 9,方法的定量限为0.2～0.5μg/kg;以猪肉、牛肉、羊肉、鸡肉、猪肝、牛肝、羊肝、鸡肝、鸡蛋和奶粉为基质,矮壮素在1.0、20.0和500.0μg/kg 3个水平下的加标回收率为84%～103%,相对标准偏差为2.13%～6.49%;对市售的271份动物源性样品进行检测,检出阳性样品26份,含量范围为1.06～14.5μg/kg。该方法简便、高效、快速、准确、灵敏度高,适用于动物源性食品中矮壮素残留的快速定量检测。     

多种香型白酒中氨基甲酸乙酯残留含量的研究

建立了液液萃取和气相色谱仪质谱联用测定白酒中氨基甲酸乙酯(Ethyl Carbamate, EC)的检测方法,该法在5～1000 ng/mL范围内线性关系良好,相关系数为R2=0.99994,在5μg/kg、25μg/kg、100μg/kg 3个水平上的加标回收率为为91.3%～105.4%,RSD为0.33%～1.90%。实际样品的测试表明,白酒基酒和市售白酒样品中EC均有检出,分别为3.01～544.74μg/kg,2.82～192.67μg/kg,市售白酒的EC平均含量为52.79μg/kg,远低于白酒基酒样品的178.90μg/kg。首次发现EC的平均含量随着白酒等级的降低而降低。     

鸡蛋中药物残留加工因子与监测结果分析

目的分析鸡蛋中药物残留膳食暴露加工因子的确定与监测样品结果。方法按监测计划采集样品并制备模拟样品,应用超高压液相色谱-串联质谱测定15种药物残留含量,并计算加工因子与去除率。结果120份样品检出氧氟沙星5份(2.5～65.8μg/kg),环丙沙星1份(2.4μg/kg)。煮蛋器15 min加工因子为0.10～0.87,微波加热(60s)加工因子为0.10～0.92。结论加工处理过程能显著降低食物中药物残留量,降低人群膳食暴露风险,蒸蛋器加热与微波烹调2种加工处理方式相比较,微波烹调过程对药物残留的去除作用小。监测结果分析表明,在不同地区、不同品种和不同参数间的药物残留检出率无统计学差异。     

中国沿海地区鸡蛋中全氟化合物污染水平及分布

为探究我国沿海地区鸡蛋中全氟化合物(perfluorinated compounds,PFCs)的污染水平及分布规律,采用分散固相萃取结合高效液相色谱-串联质谱的方法分析了我国沿海9个省/直辖市1 060份鸡蛋样品中17种PFCs的残留水平。结果表明,鸡蛋中PFCs检出率较低,均低于50%;检出的PFCs以中短链为主,占∑PFCs的82%。各省市鸡蛋样品中PFCs的残留受环境中PFCs影响较大,江苏鸡蛋样品中∑PFCs残留最高(1.24μg/kg),浙江最低(0.124μg/kg)。江苏主要全氟化合物残留为全氟辛烷磺酸(perfluorooctane sulfonate,PFOS),其他各省市为全氟戊酸。对鸡蛋中PFOS、全氟辛酸以及除此之外的短、中、长链PFCs进行风险评价,其危害指数均低于1,不具即时危害。     

陕西省生鲜乳中β-内酰胺酶的检测与结果分析

本次检测共有149份生鲜乳样品,其中鲜牛乳96份,鲜羊乳53份。旨在了解陕西省生鲜乳中是否含有β-内酰胺酶及其残留状况。采用食品整治办[2009]29号指定检验方法4《乳及乳制品中舒巴坦敏感β-内酰胺酶类物质检验方法-杯碟法》。结果共检出17份β-内酰胺酶阳性样品,阳性样品检出率为11.4%。17份阳性样品中,鲜牛乳9份,鲜牛乳阳性样品检出率为9.4%;鲜羊乳8份,鲜羊乳阳性样品检出率为15.1%。17个阳性样品的dA与dB差值较大在6.08-13.3mm。本次检测样品阳性检出率较高为11.4%,且阳性样品中所残留的β-内酰胺酶含量较高,可见生鲜乳中抗生素和β-内酰胺酶监管形势依然严峻。     

2021年吉林省20份辣条中山梨酸、苯甲酸残留量的调查分析

目的:对辣条样品中的山梨酸和苯甲酸2种防腐剂的使用情况进行统计分析.方法:运用高效液相色谱法对省内4个地级市市售的20份辣条产品中的防腐剂苯甲酸、山梨酸的含量进行检测和分析.结果:20份样品中10份样品检出防腐剂,检出率达50.0％,有9份样品中检出山梨酸,检出值为0.020～0.093 g/kg,1份样品中检出苯甲酸...     

重庆市某城区鸡蛋中指示性多氯联苯含量调查

目的了解重庆市某城区鸡蛋中多氯联苯的污染情况,为相关行政部门加强监管提供依据。方法 2014年9月在重庆市某城区辖区内随机采购鸡蛋25件样品,采用稳定性同位素稀释的气相色谱-质谱法检测其中指示性多氯联苯的含量。结果所采集的25件鸡蛋样品中,共检出2种指示性多氯联苯,其中PCB28检出4件,含量范围0.90~2.24μg/kg,PCB52检出3件,含量范围0.47~0.70μg/kg。结论重庆市某城区内销售的鸡蛋中多氯联苯类物质检出率较低,检出样品中的多氯联苯含量不高。     

市售鸡肉与鸡蛋中四环素类抗生素残留调查与膳食暴露风险评估

目的 了解杭州地区市售鸡肉与鸡蛋中四环素类抗生素残留的污染状况,探讨其污染来源,评价其膳食安全性。方法 2021年在杭州市随机抽取66份鸡肉样品和71份鸡蛋样品,采用液相色谱-质谱/质谱法监测四环素类抗生素（四环素、土霉素、金霉素和强力霉素）,采用食品安全指数来评估样品中四环素类抗生素的残留风险。结果 鸡肉中检出强力霉素与土霉素,检出率分别为45.4%和1.52%,四环素与金霉素均未检出,无超标样品;鸡蛋中强力霉素检出率与超标率均为1.41%,其余项目均未检出;鸡肉与鸡蛋中四种四环素的食品安全指数远<1,说明其污染程度对食品安全影响很小。结论 杭州地区市售鸡肉和鸡蛋中存在一定的四环素类抗生素残留,但污染程度较轻,鸡肉与鸡蛋的安全状态均为可接受。     

UPLC-MS/MS技术检测农副产品中棉酚的含量

为定量分析棉籽油、鸡蛋和牛奶中棉酚的含量,利用悬浮固化分散液相微萃取的前处理技术联合超高效液相色谱串联质谱方法,优化了悬浮固化分散液相微萃取的提取条件:采用100μL正十二烷醇作萃取剂, 100μL乙腈作分散剂,超声辅助提取30 min。用超高效液相色谱串联质谱在最优条件下进行检测,样品在三个加标浓度下加标回收率在78.25%～95.19%之间,方法的检出限(LOD)低至0.05μg/kg,定量限(LOQ)为0.167μg/kg,相关系数(R)为0.999 960, RSD均小于12.00%。对市售棉籽油、鸡蛋和牛奶中棉酚进行检测,结果显示,除从小型榨油作坊购买的棉籽油中有微量棉酚检出外,其它样品中均未检出棉酚。此方法成功应用于农副产品中棉酚的定量分析。     

气相色谱-质谱法测定植物油中壬基酚含量

目的建立气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)检测植物油中壬基酚(4-nonylphenol,4-NP)的分析方法,了解市售植物油中壬基酚的污染状况。方法样品加入乙腈提取液,超声提取、固相萃取柱净化、七氟丁酸酐衍生化后,采用GC-MS进行检测,同位素内标法定量。结果在线性范围5~200μg/kg内,方法回归方程为Y=7.78×10~(-3)X,相关系数为0.9991。方法的检出限为3.0μg/kg,定量限9.8μg/kg。加标回收率范围为75.7%~107.4%,相对标准偏差(relative standard deviation, RSD)为5.5%~9.7%。共检测50份市售植物油样品,其中26份植物油样品检出4-NP,检出率为52%,含量范围为3.21~28.2μg/kg,中位值为3.63μg/kg。结论此方法灵敏度较高,可用于植物油中4-NP的准确定量。检测数据表明,植物油样品壬基酚检出率较高,因此对其含量的监测不容忽视。     

2018年广西禽蛋中兽药残留风险检测结果分析

目的 对广西不同地区禽蛋中兽药残留水平进行测定和风险分析。方法 采集广西11个地区超市、农贸市场等各流通领域的禽蛋82批次, 按照国家标准方法和《2018年国家食品污染物和有害因素风险监测工作手册》对禽蛋中14类48种兽药残留进行检测, 检测结果依据2002年农业部235号公告《动物性食品中兽药最高残留限量》等进行评价。结果 此次风险分析, 检出有兽药残留的样本22批次, 涉及8类19种兽药残留, 检出率为26.8%。结论 目前广西禽蛋中兽药残留风险现状不容乐观, 其中磺胺类及其增效剂和喹诺酮类残留情况较严重, 硝基咪唑类、氯霉素类次之, 应该引起相关部门重视, 加强对禽蛋产品药物残留的监控。     

北京地区鸡蛋中多溴联苯醚及甲氧基衍生物污染特征及其膳食风险评估

为揭示北京地区鸡蛋中多溴联苯醚（polybrominated diphenyl ethers,PBDEs）及其甲氧基衍生物（methoxylated polybrominated diphenyl ethers,MeO-PBDEs）的污染特征,本实验利用气相色谱-负化学电离源-质谱分析了北京地区65 个鸡蛋样品中12 种PBDEs及5 种MeO-PBDEs的污染水平与组成特征。结果表明,鸡蛋中ΣPBDEs和ΣMeO-PBDEs的含量水平分别为ND（未检出）～2.21 μg/kg（以全蛋湿质量计,下同）和ND～0.89 μg/kg,检出率分别为15.38%和4.62%,与国内外相关研究相比处于较低水平。PBDEs中BDE-71的检出质量浓度较高,MeO-PBDEs以MeO-85为主要检出成分,其中蛋黄中的PBDEs和MeO-PBDEs的检出种类数量及含量均高于蛋白。通过膳食风险评估,表明北京市售鸡蛋产品中PBDEs的污染水平和膳食暴露均在可接受的范围内。     

Simultaneous Determination of 20 Inorganic Elements in Preserved Egg Prepared with Different Metal Ions by ICP-AES

In the present study, 20 inorganic elements in three parts of preserved eggs prepared with different metal ions, including Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Li, K, Mg, Mn, Mo, Na, P, Pb, Zn, Se, and Sr, were determined simultaneously by using inductively coupled plasma–atomic emission spectrometry (ICP-AES). The recoveries obtained by the standard addition method ranged between 84.4 and 112.2 %, and RSDs were lower than 8.76 %, The detection limits of the method for the 20 elements were in the range of 0.4–10 μg?L^?1. The determination results showed that three parts of preserved eggs prepared with different metal ions are all rich in essential inorganic elements, such as Na, K, P, Ca, Mg, Fe, Cu, and Zn, and the contents of most of the inorganic elements in egg yolk are higher than in egg white. In comparison with fresh duck eggs, the contents of Na, Cu, Fe, Al, and Mn are significantly increased in three parts of preserved eggs prepared with different metal ions. Metal ions added in pickling solution would significantly affect the content of element added in preserved eggs. High contents of Pb (20.15 μg/g in egg shell, 18.99 μg/g in egg white, and 0.96 μg/g in egg yolk) were found in preserved eggs with PbO. Meanwhile, the experimental results indicated that the ICP-AES technique is easy to operate, rapid, accurate, and highly sensitive to determine many inorganic elements simultaneously in preserved egg.     

Oxytetracycline residues in retail chicken eggs in Ibadan,Nigeria

Oxytetracycline residues in chicken eggs from five markets within Ibadan metropolis were determined by high-performance liquid chromatography following solid-phase extraction. Recovery of oxytetracycline was 80.5%–87.8%, whereas 75.2% of the samples contained detectable oxytetracycline with an overall mean residue concentration of 479.0?µg?kg^?1. Residue concentrations from Iwo Road, Apata, Challenge, Ojoo and Bodija markets were 421, 460, 468, 568 and 476?µg?kg^?1, respectively. Eggs from Ojoo market had the highest levels, whereas 68.8% of the samples contained residues above the Codex Alimentarius Commission maximum residue limit. The results are of public health interest as they indicate that a greater proportion of eggs being consumed in Ibadan could contain residues above the maximum residue limit, for which unregulated access and indiscriminate use of antibiotics by poultry farmers could be responsible. National surveillance of eggs and other animal products for antibiotic residue and appropriate regulation of antibiotic is recommended to ensure food safety for consumers.     

气相色谱质谱法检测鸡蛋中氟苯尼考及氟苯尼考胺

建立了气相色谱飞行时间质谱法同时检测鸡蛋中氟苯尼考和氟苯尼考胺的残留。样品经氨化乙酸乙酯提取,采用气相色谱飞行时间质谱法测定。试验结果表明:在2~100 ng/mL的范围内,线性良好,氟苯尼考R²=0.999,氟苯尼考胺R²=0.998;该方法两种物质的检出限为0.5μg/kg;在0.5、1.5、10.0μg/kg的3个水平,氟苯尼考及氟苯尼考胺的回收率在86.4%~119.4%,相对标准偏差RSD(n=3)为2.9%~7.1%,该方法简单、快速、高效,可用于鸡蛋中氟苯尼考及氟苯尼考胺的同时测定。     

Optimization of iron supplementation for enhanced detection of Salmonella Enteritidis in eggs

Mixed raw egg contents were inoculated with approximately 10 CFU of Salmonella Enteritidis and supplemented with 0 to 7 mg of FeSO4 per g of egg contents. Egg contents were then incubated at 37 degrees C, and Salmonella Enteritidis colonies were enumerated for up to 106 h. Iron supplementation significantly enhanced the growth of Salmonella Enteritidis. Within the first 24 h of incubation, the optimum iron level for Salmonella Enteritidis growth in egg contents was between 0.2 and 2 mg of FeSO4 per g of egg contents. After 24 h of incubation at 37 degrees C. Salmonella Enteritidis counts in eggs supplemented with 0.5 mg of FeSO4 per g of egg contents consistently reached approximately 1 x 10(9) CFU/ml, whereas Salmonella Enteritidis counts in eggs without iron supplementation varied from less than 5 CFU/ml to 8.4 x 10(6) CFU/ml. A 3 by 3 factorial design was used to study the effect of type of preenrichment and level of iron supplementation on the growth of Salmonella Enteritidis in egg contents. No significant differences in Salmonella Enteritidis counts between preenrichment and nonpreenrichment treatments were observed when egg contents were supplemented with 0.5 mg of FeSO4 per g of egg contents. It was concluded that preenrichment was not necessary for isolation of Salmonella Enteritidis from eggs. The effect of iron supplementation on the sensitivity of detection by the direct plating method was investigated. The direct plating method detected a significantly higher percentage of Salmonella Enteritidis in raw egg contents supplemented with 0.5 mg of FeSO4 per g of egg contents (90%) than in raw egg contents without iron supplementation (63.3%).     

紫外-可见分光光度法快速检测蛋黄中苏丹红Ⅳ的研究

采用紫外一可见分光光度计对新鲜鸭蛋蛋黄的石油醚一丙酮的提取液进行光谱扫描,建立了纯蛋黄液、标准苏丹红Ⅳ样品以及含有苏丹红Ⅳ的蛋黄液的光谱扫描曲线.通过对光谱扫描曲线的相似度比较及对光谱扫描原始曲线图的数学处理,分别运用波长差和一级微分两种方法,快速检测出新鲜鸭蛋黄中苏丹红Ⅳ.实验结果表明.波长差法的回收率高于一次微分法,而且数值分布相对集中,在对被检测样品中的苏丹红Ⅳ的定量上的精确性和稳定性优于一次微分法,而一次微分法则可直观对苏丹红Ⅳ定性.运用波长差法计算样品RSD(%),得备检样品加标苏丹红Ⅳ 2μg/mL的RSD(%)为14.2,平均回收率为106.01%,加标4μg/mL的RSD(%)为9.4,平均回收率为105.68%;运用一次微分法进行计算,得备检样品加标苏丹红Ⅳ 2μg/mL的RSD(%)为10.41,平均回收率为82.46%,加标4μg/mL的RSD(%)为6.73,平均回收率为94.21%.数据表明样品中加标苏丹红Ⅳ浓度越大.该方法对样品检测的稳定性越好.     

产前饲喂模式下恩诺沙星在初产蛋中的残留规律及膳食暴露评估

目的 消费者长期食用残留恩诺沙星的禽蛋会造成耐药性、过敏反应以及肠道菌群紊乱。本试验旨在探讨蛋鸡产蛋前喂饲恩诺沙星在初产蛋中残留规律,评估其对鸡蛋安全性以及消费者健康的影响。方法 选取378只日龄为85天的海兰褐蛋鸡,根据给药时间分为14组,1.5 g/kg恩诺沙星粉剂,连续拌料喂药 5 d。从给药后生产第 1 枚鸡蛋开始连续采集鸡蛋8天,分析鸡蛋中恩诺沙星及其代谢产物环丙沙星残留量,采用每日允许摄入量对安全性进行评估。结果 初产蛋中恩诺沙星和环丙沙星含量均随着停药时间延长逐渐降低。给药5d,停药1天的初产蛋中恩诺沙星和环丙沙星含最高分别为959.725 mg/kg和62.263 mg/kg,停药7d后鸡蛋中环丙沙星含量低于检出限,痕量恩诺沙星代谢缓慢,停药24d后鸡蛋中恩诺沙星含量低于检出限。停药1d的初产蛋对儿童和成年人身体健康具有慢性危害风险。结论 为了保证禽蛋中无恩诺沙星残留建议至少需要在产蛋前29天用药,停药24天以上,以满足产品符合国家监管以及保证消费者健康的要求。     

An automated HPLC determination of meticlorpindol in eggs with UV absorbance detection, using on-line dialysis and pre-concentration as sample clean-up; occurrence in and carry over to eggs

A fully automated HPLC determination of the coccidiostat meticlorpindol in whole egg, egg white and yolk is described. The sample homogenate is dialysed on-line against water. The dialysate is concentrated on-line on a short reversed-phase (RP) column. The contents of this column are transferred to the reversed-phase analytical column by means of the mobile phase. Meticlorpindol is detected using an absorbance detector at 270 nm. Linear calibration graphs are obtained in the range 40-900 ng/g in whole egg and egg white (detection limit 10 ng/g) and 80-1800 ng/g in yolk (detection limit 20 ng/g). Out of 111 commercially obtained egg samples 12 contained meticlorpindol with levels varying from 10 to 433 ng/g. A group of laying hens, kept in cages, received 10 mg/kg of Lerbek (meticlorpindol and methylbenzoquate; Dow Chemical) in the feed for 10 days. Meticlorpindol residues in the eggs rose to a level of 622 ng/g. Meticlorpindol was found in the eggs until 6 days after withdrawal of the medicated feed. Another group received 110 mg/kg in the feed. Meticlorpindol residues rose to levels of 4480 ng/g in the eggs, 5880 ng/g in the egg white and 2660 ng/g in the yolk. Meticlorpindol was found in the eggs and the egg white until 14 days and in the yolk until 8 days after withdrawal of the medicated feed.