QuEChERS-LC-MS/MS法快速检测鱼肉中54种兽药残留

为改进和优化鱼肉中多兽残检测的QuEChERS样品前处理方法,考察了提取剂、吸附剂以及浓缩过程对54种兽药提取回收率的影响,建立了以乙腈饱和的正己烷为分散剂,0.5%甲酸乙腈为提取剂,C18粉为吸附剂并采用稀释法减少溶剂效应的QuEChERS样品前处理方法,结合液相色谱-串联质谱（LC-MS/MS）技术可同时测定鱼肉中54种兽药残留。方法简便、快速、准确、可靠,适用于鱼肉样品中多兽药残留的快速检测。     

超高效液相色谱-串联质谱法测定水产品中50种兽药残留

目的 建立QuEChERS-超高效液相色谱-质谱/质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定水产品中50种兽药残留(三苯甲烷类、酰胺醇类、硝基咪唑类、磺胺类、喹诺酮类)的方法。方法 样品经过含1%甲酸的乙腈溶液提取, 采用QuEChERS方法净化, 通过相同C18色谱柱分离, 经2个不同流动相系统(0.1%甲酸水溶液-甲醇、5 mmol/L乙酸铵水溶液-甲醇)梯度洗脱后, 采用UPLC-MS/MS电喷雾正离子模式、正负切换模式分别分析测定, 基质添加标准曲线外标或内标法定量。结果 50种药物标准曲线相关系数均≥0.997, 检出限为0.0319~0.356 418 μg/kg, 加标回收率为60.7%~114%, 相对标准偏差为1.06%~14.1%。结论 本方法快速、高效, 可应用于水产品中多种兽药残留的快速准确筛查和检测。     

QuEChERS结合液相色谱-串联质谱法检测茶叶中34种农药残留

目的建立QuEChERS结合液相色谱-串联质谱法同时测定茶叶中34种农药残留的分析方法。方法样品加入乙腈后使用漩涡混合和超声波提取,应用QuEChERS方法进行净化处理。采用0.05%甲酸水(A)和乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多反应离子监测模式对34种农药的定量离子和定性离子进行监测。结果本方法在17 min内完成34种目标化合物的分离分析。34种农药在2.5～200μg/L范围内线性关系良好,相关系数(r)均大于0.995,方法的定量限为0.01～5.11μg/kg。34种农药在20、50和100μg/kg添加水平的回收率为70.6%～116.1%,相对标准偏差为1.0%～8.1%(n=6)。结论该方法简单、快速、准确、灵敏高,适合用于茶叶中农药多残留的测定。     

QuEChERS结合液相色谱串联质谱法同时测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留

目的建立液相色谱-串联质谱法测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留的分析方法。方法样品经乙腈提取,QuEChERS法进一步净化,离心后取上清液用氮气吹至近干,残渣用初始流动相溶解。用5 mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱,Poroshell 120 EC-C_(18)色谱柱进行色谱分离,使用电子喷雾离子源(electron spray ionization,ESI-)和选择反应监测(selected reaction monitoring,SRM)模式测定,初始流动相配制标准曲线,外标法定量。结果本方法在8 min内完成7种目标化合物的分离分析。7种农兽药在1～50μg/L范围内具有较好的线性关系,相关系数均r~2大于0.996。回收率在82.7%～117.8%之间,相对标准偏差小于9.9%(n=6)。结论该方法样品前处理简单、效率高、灵敏、可靠、适用测定鸡蛋中氟虫腈与氯霉素等7种农兽药残留。     

QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留

目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0 g用乙腈-水(4:1)15 mL超声提取,经N-丙基乙二胺(PSA)30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5~200 μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3 μg/kg。加标回收率84.3%~102%,相对标准偏差(n=6)2.8%~6.3%。结论:该方法可用于食用菌中13种农药残留的检测。     

液相色谱-串联质谱法快速检测大米中的15种农药残留

目的建立液相色谱-串联质谱法快速检测大米中15种代表性农药残留的分析方法。方法大米样品经水溶胀后以乙腈提取,利用QuEChERS法进行净化。采用0.02%甲酸+2 mmol/L甲酸铵(A)和甲醇(B)作为流动相进行梯度洗脱,采用多离子监测模式对农药多残留进行检测。结果在9.5min内完成15种目标农药残留的分离分析。在0.010、0.10和0.50mg/kg3个添加水平的回收率为70.2%～110.0%,相对标准偏差为1.3%～14.5%(n=3);方法定量限为0.010 mg/kg、检出限为0.2～1.0μg/kg。结论该方法简便、快速、准确、实用,适合测定大米样品中的农药残留。     

PRiME HLB固相萃取-高效液相色谱-串联质谱法同时快速测定鸡蛋中48种兽药残留

建立固相萃取-高效液相色谱-串联质谱同时快速测定鸡蛋中48种兽药残留的分析方法。样品采用90%乙腈水溶液提取,用PRiME HLB小柱净化浓缩后用电喷雾离子源,正负离子扫描,多反应监测模式的高效液相色谱-串联质谱法进行检测,以基质匹配曲线外标法定量。正离子采用CAPCELL PAK C18 MGⅢ-H色谱柱,流动相为0.05%甲酸乙腈和0.1%甲酸水;负离子采用ACQUITY UPLC BEH C18色谱柱,流动相为5 mmol/L乙酸铵和乙腈。结果表明,鸡蛋样品中的48种兽药残留在0.5~50 μg/kg浓度范围内线性关系良好,相关系数(r)为0.9952~1.0000。方法检出限为0.01~0.55 μg/kg,定量限为0.03~1.83 μg/kg,样品回收率在63.3%~111.4%之间,相对标准偏差小于10%(n=3)。本方法操作快速简单,重复性好,灵敏度较高,适用于鸡蛋中48种兽药残留的快速筛查检测。     

QuEChERS -超高效液相色谱串联质谱法快速测定禽蛋中7种喹诺酮类兽药残留

建立一种超高效液相色谱串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定禽蛋中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星和沙拉沙星共7种喹诺酮类兽药残留的分析方法。禽蛋样品经体积分数为5%的甲酸-乙腈提取喹诺酮类兽药残留,QuEChERS净化后通过快速溶剂蒸发系统浓缩,采用C_(18)色谱柱分离,以体积分数为0.1%的甲酸和乙腈为流动相进行梯度洗脱,电喷雾离子源电离,多反应监测模式采集信号,基质外标法定量。结果表明,7种喹诺酮类兽药在2.0～100.0 ng/mL线性关系良好(R~2>0.995),方法的检出限和定量限分别为0.3和1.0μg/kg;添加2、5、10μg/kg三个浓度水平,平均回收率为77.20%～98.47%,相对标准偏差为1.5%～6.2%(n=6)。该方法简单快捷、准确度好、灵敏度高,适用于禽蛋中喹诺酮类兽药残留的快速确证。     

超高效液相色谱-串联质谱法检测植物源加工食品中农药残留

目的 建立植物源性预包装食品中35种农药残留的超高效液相色谱-串联质谱检测方法。方法 样品经乙腈提取,QuEChERS方法净化,经Shim-pack GIST C18色谱柱分离,以乙腈和0.1％甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)/负离子(ESI-)模式电离,MRM扫描模式检测。结果 经方法学验证,本方法的线性关系、回收率、精密度均符合要求。结论 可实现植物源性预包装食品中35种农药残留的同时定性、定量分析。本方法重现性好,回收率高。     

三重四极杆气相色谱质谱联用法测定茶叶中31种农药残留

目的 建立一种简便、快速、安全、价格低廉的三重四级杆气相色谱质谱联用仪法(QuEChERS-GC-MS/MS)测定茶叶中的31种农药残留的分析方法。方法 以0.5%的乙酸-乙腈(v/v)溶液作为溶剂,以加入无水硫酸镁、醋酸钠进行浸提,浸提后用硅酸镁、乙二胺-N-丙基硅烷化硅胶(PSA)、C18和石墨化炭黑(GCB)净化试剂净化,净化液用氮吹仪浓缩至干,用0.5%的乙酸-乙腈定容至,采用内标法定量,气相色谱-质谱联用仪(GC-MS/MS)同时测定31种农药残留。结果 31中农药的线性相关系数达到0.999以上,检测限(LOD)为0.01~0.05mg/kg。同时采用红茶和绿茶作为基质本底, 用加标回收评价了该方法的精密度和重现性,31种农药的平均回收率为85%-105%,相对标准偏差为0%-10%。结论 该方法操作简便快捷、检测成本低,方法的灵敏度、准确度和精密度符合茶叶中农药残留测定的技术要求。 关键词: QuEChERS; 三重四级杆气相色谱质谱联用仪; 农药残留; 茶叶     

免疫分析技术在食品农残药残检测方面的应用

介绍了酶免疫分析技术的简单分类;并叙述了酶免疫技术、放射免疫技术、金免疫技术等免疫学分析技术在食品中农药残留、药物残留检测方面的应用。     

Determination of tetracycline residues in chicken meat by liquid chromatography-tandem mass spectrometry

Analysis of residual levels of tetracyclines (TCs) in chicken meat was performed using a validated liquid chromatography coupled with a tandem mass spectrometry (LC-MS/MS) technique. Overall, the recoveries for TCs ranged from 56.9% to 101.2%, with standard deviations of 4.5–13.2%. Detection limits ranged from 7.9 to 14.6?µg?kg^?1. In four of 60 samples, doxycycline (DXC) was determined in a range from 19.9 to 35.6?µg?kg^?1; and in one sample tetracycline was detected at 17.2?µg?kg^?1. Chlortetracycline (CTC) and oxytetracycline (OTC) were not detected in any of the tested samples. This study indicates that chicken meat sold in Bursa, Turkey, contained some residues of TCs. Therefore, stricter regulations for the use of antibiotics in the poultry industry and the monitoring of drug residues in chicken meat prior to marketing are needed. Finally, this method has been applied successfully for the confirmation of TCs in chicken meat.     

2010年深圳某高校蔬菜中有机磷及氨基甲酸酯类农残的检测分析

通过抽样检测深圳市某高校饭堂采购的蔬菜瓜果中有机磷及氨基甲酸酯类农药残留的情况,为该校监管蔬菜质量提供科学数据.数据表明,叶菜类较瓜果类蔬菜较为容易超标,瓜果中超标样品多见于茄瓜、苦瓜、云南小瓜及青瓜.结果显示:农残检测未超标率(即合格率)为91.1%,农残超标率为5.3%,可疑农残超标率为3.6%.这为蔬菜质量的把关...     

茶叶农药残留检测中咖啡因干扰的去除

用热水(45℃)＋有机溶剂(二氯甲烷)的提取法,结合Carbosil 小柱(用于有机磷农残)和Florisil 柱(用于菊酯类农残)净化处理,除去茶叶中的咖啡因对农药残留检测的干扰;对茶叶中常检农药残留如拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、氰戊菊酯 、氯氰菊酯、溴氰菊酯等) 和有机磷农药( 滴滴畏、乐果、甲基对硫磷、喹硫磷、三唑磷等)在三个加标水平0.2、0.8、1.6mg/kg 上进行了方法的单实验室验证。结果表明：本前处理方法能有效去除茶叶中咖啡因对农药残留检测的干扰;对上述有机磷农残各加标水平上的平均回收率在73%～112.9% 之间,RSD<8%,最低检出限在0.002～0.02mg/kg;对上述菊酯类农残各加标水平上的平均回收率在78.8%～105% 之间,RSD<9%,最低检出限在0.001～0.006mg/kg,均符合或优于我国和欧盟有关法规的规定。     

Development of an enhanced histopathological approach to detect low-dose dexamethasone illicit treatment in veal calves

Dexamethasone is one of a number of synthetic corticosteroids illegally used to promote growth in food-producing animals. Since these low-level drug cocktails evade detection by currently available chemical methods, simple biological indicators that can aid in laboratory analysis are needed. In an attempt to devise an accurate biological method that could detect illicit drug treatment in food-producing animals, we characterized microscopic morphologic alterations of the thymus in veal calves administered low-dose dexamethasone versus control animals. For this purpose, 122 male calves were farmed for 6 months in controlled condition: 81 animals were orally administered dexamethasone (0.4?mg?day^?1) for 20 days during the sixth month and the remaining 41 were kept as control. Urine samples were collected systematically during the treatment period, the suspension period and at the slaughterhouse. All animals were slaughtered 10 per day starting from 10 days after the last dexamethasone administration and the thymus was sampled for histological examination. The difference between the two animal groups was evaluated by means of a non-parametric test of hypothesis. No residues were detected in the urines collected since the third day after the last administration, whereas morphometric analysis of the thoracic thymus revealed a significant decrease in the cortex:medulla ratio in the treated animals (p?<?0.0005). We can conclude that this histological approach offers encouraging prospects as a screening method to overcome current limitations in controlling growth promoter abuse.     

QuEChERS法在食品有机污染物检测中的研究进展

食品中的农药残留、真菌毒素、兽药残留等有机污染物是危害食品安全的主要因素之一,因此,建立食品中多种有机污染物的高效提取和净化方法对于快速了解食品中有机污染物含量、保障食品安全具有十分重要的意义。本文在介绍QuEChERS(quick,easy,cheap,effective,rugged and safe)法及其近年来在食品有机污染物检测中的应用基础上,对其在应用过程中存在的问题进行了系统分析,提出该方法优化的一般思路,并展望了该方法在食品有机污染物检测中的未来发展趋势。     

Validation of a commercial receptor kit Sulfasensor® Honey for the screening of sulfonamides in honey according to Commission Decision 2002/657/EC

The Sulfasensor® Honey kit is a receptor test dedicated to the screening of sulphonamide residues respectively in different matrices. The aim of this project was to evaluate and validate this kit according to the Community Reference Laboratory (CRL) guideline for the validation of screening methods to achieve the French control plan for honey. The test is robust, quick (90?min for 40 samples), easy to perform and easy to read. The false-positive rate was estimated to be 12.5%. The detection capabilities CCβ of the kit were lower than or equal to 25?µg?kg^?1 for sulfamethazine, sulfamerazine, sulfathiazole and sulfapyridine, and between 25 and 50?µg?kg^?1 for sulfadiazine and sulfadimethoxine, 150?µg?kg^?1 for sulfaquinoxaline, and 1000?µg?kg^?1 for sulfamethoxazole and sulfamethizole. Sulfanilamide was not detected by the kit. The kit was applicable to a wide variety of honeys (different floral and geographical origins, liquid or solid). This kit was used to implement the French control plan for the detection of antibiotic residues in honey in 2010 in parallel with an HPLC method. However, in 2011 the kit was replaced by an LC-MS/MS method for the screening and confirmation of sulfonamide residues in honey, which detects all the sulfonamides of interest.     

高效液相色谱法测定畜、禽肉中土霉素的残留量

土霉素属抗生素类药物,无公害食品标准规定应在0.1 mg/kg以下.按GB/T5009.116-2003国家推荐方法检测,方法检出限为0.15 mg/kg,很难满足判定要求.本文通过优化条件,摸索出一个简捷、快速、经济,又能保证一定精度的测定方法来满足分析要求.本方法加标回收率在96.0%～108.2%之间,线性系数R=0.9999,检出限0.08 mg/kg,分析时间仅为9 min,完全能够满足分析要求,具有广泛的应用前景.     

食品加工过程对食品中的农药残留的影响

食品加工过程是农产品深加工的重要环节,涉及的加工方式多--清洗、去皮、榨汁、制酱、蒸煮,本文综述了这些过程对食品中农药残留的影响。     

Survey of 11 nitroimidazole residues in hen and duck eggs from the Irish market

A liquid chromatography–tandem mass spectrometry method, recently developed, validated and accredited, was used to screen for metronidazole, ronidazole dimetridazole ipronidazole, ternidazole, tinidazole, ornidazole carnidazole and three hydroxy metabolites (hydroxy-metronidazole, HMMNI and hydroxy-ipronidazole) in Irish retail egg samples. The method used had decision limits (CCα) in the range 0.33–1.26?µg?kg^?1 and detection capabilities (CCβ) ranging 0.56–2.15?µg?kg^?1 for all analytes. Internal standard-corrected recovery, calculated for the various analytes, ranged 87.2–106.2%, while the coefficient of variance, expressed as % CV, ranged 3.7–11.3%. The method was applied to 160 samples of caged, free range and organic hen and duck eggs available on the Irish retail market as well as two incurred proficiency test egg samples. No nitroimidazole residues were detected in the survey samples above the CCα and the results achieved for the two proficiency test samples were acceptable when compared with the assigned values.