湖北省鸡肉和鸡蛋中多组分抗生素残留分析

目的 了解湖北省鸡肉和鸡蛋中喹诺酮类、四环素类抗生素和甲硝唑残留水平。方法 依据《国家食品污染和有害因素风险监测工作手册》中样本采集要求,2016—2019年湖北省采集373份鸡肉和365份鸡蛋,利用超高效液相色谱-串联质谱法（UPLC-MS/MS）检测9种喹诺酮类、4种四环素类抗生素和甲硝唑残留水平。结果 2016—2019年检测的鸡肉和鸡蛋样品中分别有65件和50件检出抗生素残留。鸡肉中抗生素年度检出率分别为9.76%（8/82）、16.67%（16/96）、38.14%（37/97）、4.08%（4/98）,鸡蛋中抗生素年度检出率分别为15.00%（12/80）、8.24%（7/85）、24.00%（24/100）、7.14%（7/98）,4个年度鸡肉和鸡蛋中抗生素检出率均有显著性差异（χ²=44.454,P<0.001;χ²=14.730,P=0.002）,不同采样环节抗生素的检出率没有统计学差异（χ²=0.053,P=0.819）,鸡蛋中检出有强力霉素、恩诺沙星、环丙沙星、甲硝唑、氧氟沙星、诺氟沙星等禁用抗生素,同时鸡肉中也检出了甲硝唑。结论 鸡肉中喹诺酮类和四环素类抗生素检出率较高,残留水平较低,但鸡肉和鸡蛋中非法使用的禁用抗生素会给人群带来健康风险不容忽视。     

超临界色谱串联静电场轨道阱质谱法测定蔬菜水果中高极性农药残留

目的 建立基于超临界色谱技术（SFC）结合静电场轨道阱质谱法（Q-Orbitrap）对蔬菜水果中12种高极性农药残留量的测定方法。方法 样品用1%酸化甲醇提取,提取液经分散固相萃取净化,以Ultra Silica柱（150 mm×2.1 mm, 3 μm）和Obelisc R柱（150 mm×2.1 mm, 5 μm）为分离柱,使用超临界色谱-串联静电场轨道阱质谱（SFC-Q-Orbitrap）测定,以分段式混合产物离子扫描,采用同位素内标校准曲线定量。结果 12种农药在20.0～500 μg/L范围内线性关系良好,决定系数（R²）均＞0.997,在0.05、0.20 mg/kg 2个加标浓度下的平均回收率为80.2%～120%,相对标准偏差（RSD,n＝6）为2.14%～14.6%,方法的检出限为0.010 1～0.016 2 mg/kg,定量下限为0.050 mg/kg。结论 方法具有操作简单、专一性强、定量准确、测定高效等优点,经实际样品测试,可满足蔬菜水果中高极性农药残留的检测。     

安徽省鸡肉、鸡蛋和鸡内脏中重金属污染状况调查分析

目的 研究安徽省鸡肉、鸡蛋和鸡内脏组织中的重金属的污染状况,为食品安全风险监测、引导饮食提供一定依据。方法 随机采集2019年安徽省各地市鸡肉、鸡蛋、鸡肝和鸡胗样品,检测重金属元素砷（As）、铅（Pb）、镉（Cd）、铬（Cr）、汞（Hg）的含量,并结合中国居民食物消费量调查数据,将居民膳食中各重金属暴露量结合健康指导值进行简单分析。结果 此次研究的鸡肉、鸡蛋、鸡肝、鸡胗样品各重金属检出率不同,合格率为100%;同一重金属元素（除Pb外）在鸡肉、鸡蛋、鸡胗和鸡肝中含量差异均具有统计学意义（P<0.05）,不同重金属元素的含量差异有统计学意义（χ²=17.13,P<0.05）;重金属在内脏中含量高于鸡肉和鸡蛋,其中Cr含量最高,Pb次之;安徽省人群鸡肉、鸡蛋和鸡内脏中各重金属暴露量远低于其健康指导值。结论 安徽省鸡肉、鸡蛋和鸡内脏对重金属元素的累积能力不同,重金属在内脏中更容易累积,安徽省鸡肉、鸡蛋和内脏中重金属的含量较低,人群膳食暴露量较低,对人体健康产生危害的风险相对较小。     

2016—2020年天津市市售蔬菜中农药残留状况及膳食暴露评估

目的 了解天津市市售蔬菜中农药残留状况及居民膳食暴露风险。方法 根据《国家食品污染物及有害因素风险监测工作手册》要求,采集代表性时令蔬菜516份进行农药残留量检测,利用点评估方法对其进行膳食暴露评估。结果 70.54%（364/516）样品检出农药残留,其中47.29%（244/516）样品同时检出2种或以上农药;6.01%（31/516）样品农药残留量超标。各类型农药超标率排序为：有机磷类农药>氨基甲酸酯类农药>拟除虫菊酯类农药>有机氯类农药>杀菌剂类农药,差异有统计学意义（χ²＝9.84,P<0.05）。超标率位于前三位的农药分别为甲拌磷（2.62%,10/381）、克百威（1.55%,8/516）和氯氰菊酯（0.90%,2/223）。急性膳食暴露评估结果,甲拌磷急性膳食摄入风险值（%ARfD）为238.89%,克百威%ARfD为191.67%,大于100%,存在不可接受的风险;慢性膳食暴露评估结果,所有检出农药单项食品安全指数值（IFS）均小于1,风险可以接受。结论 天津市市售蔬菜中农药检出率较高,尤其是多种农药联合使用的现象突出,且仍存在使用禁用农药的情况,甲拌磷、克百威存在急性膳食暴露风险,政府和相关部门应加强对此类农药的监管。     

河南省市售鸡肉中抗生素残留及大肠埃希菌耐药性研究

目的 了解河南省市场零售环节冰/鲜鸡肉中抗生素残留以及大肠埃希菌抗生素敏感性,为食品风险评估提供数据支持。方法 2020年5—11月对河南省零售环节采集的60份冰/鲜鸡肉采用高效液相色谱质谱串联法进行抗生素残留试验;鸡肉中分离的300株大肠埃希菌采用微量肉汤稀释法进行抗生素敏感性试验。结果 抗生素残留均未检出。300株大肠埃希菌对亚胺培南（IPM）全部敏感,其余14种抗生素耐药率范围为8%~86.33%,耐药率≥50%的抗生素有：四环素（TET）86.33%（259/300）,氨苄西林（AMP）69.00%（207/300）,氯霉素（CHL）63.33%（190/300）,头孢唑啉（CFZ）50.67%（152/300）,萘啶酸（NAL）50.00%（150/300）。多重耐药菌（MDRO）检出率高达81.75%（224/274）。地区间耐药率存在显著性差异（χ²=31.331,P<0.05）。耐药菌谱型分散,以四环素（TET）耐药谱占比最高,为8.39%（23/274）。结论 2020年河南省市场零售环节鸡肉中抗生素残留符合相关法规。鸡肉源大肠埃希菌呈现高度耐药,MDRO现象普遍,需加强规范禽类饲养环节抗生素的合理使用。     

表面增强拉曼光谱法快速检测茶叶中百草枯与敌百虫农药残留

目的 对茶叶中的百草枯与敌百虫进行定性与定量检测,满足茶叶生产中对这两种农药残留的快速、便携、准确的检测需求。方法 采用表面增强拉曼光谱(surface enhanced Raman spectroscopy SERS)技术对不同浓度的百草枯和敌百虫农药标准溶液进行光谱采集和峰位归属,再对不同茶类茶汤中的梯度农药残留进行检测,建立峰强与农药残留浓度的线性关系。结果 发现在不同茶类中,以茶叶中百草枯在843 cm_^-1处的拉曼特征峰作为识别峰所建立回归模型预测的百草枯在绿茶、红茶、黑茶茶汤中的最低可检测浓度为1×10_^-7 moL/L,在乌龙茶茶汤中的最低可检测浓度为1×10_^-6 moL/L,灵敏度均满足国家规定的茶叶中百草枯最大农药残留限量(0.2 mg/kg);敌百虫的检测中,茶汤中咖啡碱的SERS峰强受敌百虫浓度影响,随敌百虫浓度的增加而减小且呈现显著负线性相关,因此可用茶叶中咖啡碱的拉曼特征峰作为敌百虫浓度的间接识别的依据,所建立的回归模型显示敌百虫在绿茶、红茶、乌龙茶茶汤中的最低可检测浓度为1×10_^-7 moL/L;在黑茶茶汤中的最低可检测浓度为1×10_^-6 moL/L,均可达到国家茶叶最大残留限量(2 mg/kg)。结论 使用SERS技术可实现不同茶类茶汤中的百草枯与敌百虫农药残留的简单、快速、准确分析。     

分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量

目的：评估液态乳中农药残留量的安全性。方法：建立同时测定11种农药残留的超高效液相色谱—串联质谱法。待测样品经乙腈提取，C₁₈和PSA固相萃取剂净化，经色谱柱Xbridge BEH C₁₈ （100 mm×2.1 mm，1.7 μm）分离，多反应监测模式进行测定，并使用响应曲面法优化前处理参数。结果：前处理的最佳条件为乙腈用量10 mL，C₁₈用量50 mg，PSA用量30 mg。11种农药在1.0~100.0 μg/L的浓度范围内线性关系良好，相关系数（R²）均＞0.999。在10，20，100 μg/kg添加水平内，11种农药的平均回收率为82.7%~102.0%，相对标准偏差为2.89%~8.87%，检出限和定量限分别为2.0~3.0，5.0~10.0 μg/kg。结论：该方法操作简便，分析时间短，回收率高，重现性好，能够准确定性定量分析液态乳中11种农药残留量。     

广东省本地产茶叶农药多残留累积风险评估

目的 针对广东省本地产茶叶中13种常用农药,评估其慢性和急性膳食摄入风险,以期为生产监管、消费和制修订限量标准提供依据和技术支撑。方法 采集2017—2020年广东省本地产茶叶110份,按照GB 23200.113—2018方法对13种农药进行残留检测,运用危害指数（HI）法评价其急性和慢性膳食摄入风险及其累积暴露风险。结果 共检出8种农药残留,其中联苯菊酯、甲氰菊酯和氯氰菊酯检出率和残留水平最高,该3种农药广东省居民茶叶慢性和急性累积摄入量分别为4.87×10^-5 mg/（kg bw·d）和4.79×10^-3 mg/（kg bw·d）,分别占总农药摄入量的89.09%和86.01%,且均呈现男性高于女性、城市居民高于农村居民的规律。基于累积风险考虑,所有检出农药的慢性和急性累积摄入HI分别为3.69×10^-3和4.66×10^-1,摄入风险较低。结论 广东省居民通过本地产茶叶导致的多组分农药慢性和急性摄入风险低,但广东省本地产茶叶中农药残留现象普遍,应进一步加强规范农药在茶叶中的使用和管理。     

水果中26种有机氯及拟除虫菊酯农药残留GC-ECD测定

利用气相色谱(GC)建立了水果中26种有机氯农药同时测定的方法。试样中农药残留在超声波振荡条件下用乙腈提取,经PSA、C18净化,GC-电子捕获检测器(ECD)检测。方法的检出限为0.001～0.005mg/kg,回收率为84.5%～104.5%,相对标准偏差为1.1%～6.7%。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。     

NY/T 761—2008和QuEChERS前处理技术在有机氯农药检测中的应用

本研究分别采用NY/T 761—2008和QuEChERS前处理方法,结合GC-ECD应用于蔬菜和水果产品中16种有机氯农药残留的检测。结果显示:采用QuEChERS方法处理后的样品,测定结果具有良好的线性关系,平均回收率、相对标准偏差、检出限均符合农药残留测定的国家标准要求。证明QuEChERS前处理方法快速,简便,有效。     

Organochlorine pesticide residues in poultry feed,chicken muscle and eggs at a poultry farm in Punjab,India

Animals intended for human food may absorb pesticides from residues in their feed, water or during direct/indirect exposure in the course of pest control. The objective of the present investigation was to monitor organochlorine pesticide residues in poultry feed, chicken muscle and eggs at a selected poultry farm. The samples were Soxhlet extracted for 8 h in 200 mL hexane–acetone (1:1, v/v) mixture. The clean‐up of the samples was performed by silica gel column chromatography and analysis was done on a gas chromatograph equipped with an electron capture detector. The mean total hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT), endosulfan sulfate and heptachlor epoxide residues were 0.65, 0.91, 0.42 and 0.02 mg kg^?1, respectively, in feed while respective values for chicken muscle were 0.11, 0.24, 0.10 and 0.07 mg kg^?1. Higher residues were encountered in eggs as compared to muscle. None of the muscle samples exceeded maximum residue limits (MRL) for organochlorine pesticides, while all egg samples had values above the MRL for HCH and heptachlor epoxide and seven egg samples exceeded MRL for DDT residues. The results indicated that poultry feed could be one of the major sources of contamination for chicken and eggs. These residues are present despite complete ban on the use of technical HCH and DDT for agricultural purposes in India. Copyright © 2005 Society of Chemical Industry     

Organochlorine pesticide residues in domestic fowl (Gallus domesticus) eggs from central Kenya

In 367 domestic fowl (Gallus domesticus) eggs collected from 61 farms, residues of 10 pesticides were detected in various combinations and in the following order of frequency: p,p′-DDE (in 100% of the eggs), p,p′-DDT (98%), dieldrin (95%), Indiane (66%), p,p′-DDD (46%), o,p′-DDT (17%), β-HCH (9%), γ-HCH (5%), endrin (4%) and aldrin (0–5%). No residues of heptachlor, heptachlor epoxide, HCB or PCBs were found. The mean concentration (0–70 mg kg^?1 eggs; range <0–01–10–25) of total DDT exceeded the extraneous residue limit (ERL) of 0–50 mg kg^?1. The mean dieldrin residue level (0–35 mg kg^?1; range 0–01–14–90) was 3–5 times higher than the ERL (0–10 mg kg^?1). Only 3% of the eggs exceeded the ERL for Indane. The 156 eggs from free-range hens had significantly (P<0–05) higher residue concentrations of total DDT, dieldrin and Iindane than eggs collected from hens kept in enclosures. The mean ratio [p,p′-DDT]/[p,p′-DDE] in eggs from enclosed hens (0–97) was significantly higher (P<0–01) than in eggs from free-range hens (0–53), indicating that the former had a more direct exposure to p,p′-DDT, whereas the latter obtained more of it after environmental conversion to p,p′-DDE. Eggs from a rice-growing area had the highest concentrations of all pesticide residues detected. Accumulation ratios indicated that the levels of DDT and Iindane in the feed of enclosed hens could account for the levels in the corresponding eggs. The much higher accumulation ratios calculated for the free-range hens demonstrated that the feed ingested by these chickens obviously contained ingredients additional to those sampled, and revealed probable extensive environmental contamination by these persistent pesticides. The present results indicate that there is a need to identify sources of dieldrin in the eggs of domestic fowls and, where necessary to investigate local wildlife samples. The amounts of total DDT and dieldrin in eggs in this study seem to be higher than reported from any other country. Toxicological evaluation of the results indicates that, at lest in parts of KEnya there is a need for improved practices in the use of some organochlorine pesticides.     

Analysis of contaminated milk with organochlorine pesticide residues using gas chromatography

Milk and milk products are considered to have tremendous nutritional values as they contain a good proportion of protein, fats, and important minerals. However, the nutritional value of the milk produced in Pakistan is not up to the mark as extensive use of pesticides on crops resulted in contamination of milk. Consumption of contaminated food such as milk, meat, fish, eggs can induce increased proportion of organochlorine pesticides in the body. The purpose of this study is to determine organochlorine pesticide residues in milk and their toxicity level by Maximum Residues Level (MRL) values. In the current study, organochlorines such as Dichlorodiphenyltrichloroethane (DDT), Dichlorodiphenyldichloroethane (DDE), Dieldrin, Gamma-hexachlorocyclohexane (?-HCH) also known as Lindane, α-Endosulphan, β-Endosulphan and Endosulphan sulphate were detected with the help of gas chromatograph equipped with electron detector. These pesticides were confirmed by using gas chromatography-mass spectrometry (GC-MS). Analysis of variance is applied (ANOVA) to determine variations of pesticides in all milk samples. Analysis showed non-significant results (p > 0.05) with large variation among all milk samples regarding pesticide residues. The mean values of DDT, DDE were found to be below the MRL value. The mean values of Dieldrin, ?-HCH were also below MRL value. On the other hand mean values of α-Endosulphan, β-Endosulphan, and Endosulphan sulphate were slightly higher than MRL in few milk points. The present study showed large variations of pesticides residues present in milk samples.     

Assessment of average exposure to organochlorine pesticides in southern Togo from water,maize (Zea mays) and cowpea (Vigna unguiculata)

Drinking water, cowpea and maize grains were sampled in some potentially exposed agro-ecological areas in Togo and analysed for their contamination by some common organochlorine pesticides. A total of 19 organochlorine pesticides were investigated in ten subsamples of maize, ten subsamples of cowpea and nine subsamples of drinking water. Analytical methods included solvent extraction of the pesticide residues and their subsequent quantification using gas chromatography-mass spectrometry (GC/MS). Estimated daily intakes (EDIs) of pesticides were also determined. Pesticides residues in drinking water (0.04–0.40 µg l^?1) were higher than the maximum residue limit (MRL) (0.03 µg l^?1) set by the World Health Organization (WHO). Dieldrin, endrin, heptachlor epoxide and endosulfan levels (13.16–98.79 µg kg^?1) in cowpea grains exceeded MRLs applied in France (10–50 µg kg^?1). Contaminants’ levels in maize grains (0.53–65.70 µg kg^?1) were below the MRLs (20–100 µg kg^?1) set by the Food and Agriculture Organization (FAO) and the WHO. EDIs of the tested pesticides ranged from 0.02% to 162.07% of the acceptable daily intakes (ADIs). Population exposure levels of dieldrin and heptachlor epoxide were higher than the FAO/WHO standards. A comprehensive national monitoring programme on organochlorine pesticides should be undertaken to include such other relevant sources like meat, fish, eggs and milk.     

鸡肉中24种有机氯农药残留的测定方法

建立了凝胶渗透色谱前处理,毛细管气相色谱测定鸡肉中24种有机氯农药的方法。所使用的方法能使农药的提取和分配一次完成,凝胶渗透色谱柱使鸡肉中的农药与脂肪等得到较好分离,在此条件下干扰物得到了很好的去除,并提高了分析速度。在给定的浓度范围内,各农药组分呈现良好的线性相关,加标回收率在87.87%～126.34%,相对标准偏差<12.48%。方法快速、简便,适用于鸡肉中有机氯农药的快速检测。     

Pesticide residues in apples grown under a conventional and integrated pest management system

This paper describes method validation for determination of more than 40 pesticides in apples using a GC technique. Target compounds belonged to the organochlorine, organophosphorus, carbamates, pyrethroids, triazoles, dicarboximides and strobilurins groups, among others. Sample preparation consisted of acetone extraction and subsequent cleanup/concentration by SPE with a polymer-based sorbent. Single quadrupole GC–MS operating in SIM mode and electron impact ionization was used for identification and quantification of the pesticides. Average recoveries for analytes ranged between 70 and 110% at three fortification levels – 0.01, 0.1 and 0.2 mg kg^?1. Relative standard deviations were lower than 20% for all tested compounds. Calculated limits of detection and limits of quantification were below 0.01 mg kg^?1, which were sufficiently low compared to the maximum residue levels (MRLs) established by European legislation. The proposed method was applied for determination of pesticide residue in four selected apple varieties after harvesting. Whole and processed fruits (peel and peeled fruits) were analyzed from different treatment systems: two conventional, one based on integrated pest management (IPM) and two variants based on organic production (controls). Higher levels of pesticide residues were found in apple fruits under conventional conditions. Fenitrothion and chlorpyrifos residues were detected frequently in apple peel at concentrations up to 0.45 and 0.77 mg kg^?1, respectively. The levels found in the whole fruits of the same samples were much lower than in peel and below the respective MRLs (0.5 mg kg^?1 for both pesticides). Measurable residues of triadimenol only, up to 0.05 mg kg^?1, concentrated in the peel, were found in the apples from IPM.     

大米中28种有机氯及拟除虫菊酯农药残留GC-ECD测定

利用气相色谱(GC)建立了大米中28种有机氯农药及拟除虫菊酯类农药同时测定的方法。试样中农药残留在超声波振荡条件下用乙腈提取,经佛罗里硅土和PSA净化,GC-电子捕获检测器(ECD)检测。方法的检出限为0.001～0.025mg/kg,回收率为84.5%～104.5%,相对标准偏差为1.1%～6.7%。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。     

2001 survey of organochlorine pesticides in retail milk from Beijing, P R China.

A monitoring study was conducted in 2001 to determine the organochlorine pesticides and their metabolite residues in milk taken from supermarkets in Beijing, P. R. China. The average concentrations of total HCH and DDT were 0.038 and 0.046 mg x kg(-1), respectively, expressed on a fat basis. The aldrin residue was detected in nine milk samples, with a mean concentration of 0.035 mg x kg(-1). Heptachlor and its epoxides were not found in any milk samples. Of 72 milk samples analysed, three from South China contained the higher levels of DDT and HCH residues that exceeded the FAO/WHO accepted tolerance level. Although organochlorine pesticides such as DDT and HCH have been banned in China since 1983, the residues of such compounds still exist in the environment and cause food contamination, a fact likely attributed to the short prohibition period and illegal use for agricultural purposes at present.     

Performance comparison of free and immobilised chicken liver esterase inhibited by four different pesticides

BACKGROUND: In enzyme inhibition‐based biosensors for the detection of organophosphate and carbamate pesticides, the biological element is the immobilised esterase which is inhibited selectively by the pesticides. The free chicken liver esterase, which possesses comparable inhibition response to the pesticides as AChE, has been reported. However, the responses to the pesticides are different between the free and immobilised enzyme due to the diffusion limitation. Therefore, in this study four typical pesticides were selected to compare the ability of free and (ion exchange) immobilised chicken enzyme for pesticide detection and reasons for the difference were investigated. RESULTS: For dichlorvos and malathion at a concentration of 0.1 mg L^?1, the inhibition of the immobilised enzyme was 26.98% and 48.72%, respectively, higher than that for the free enzyme, while the percentage inhibition of free and immobilised enzyme differed very little for trichlorfon at 0.1 mg L^?1. In the meantime, carbaryl at a concentration of 2.5 mg L^?1 showed a 17.72% inhibition for immobilised enzyme which was 13.64% higher than that for the free enzyme. The Michaelis constant of immobilised enzyme was lower than that of the free one and suitable pH values for the free and immobilised enzyme were 7.5 and 8.0, respectively. CONCLUSIONS: The sensitivity of chicken liver esterase to the pesticide inhibition could be improved by immobilisation. Smaller K_m and a lower pH for the micro‐environment of immobilised enzyme should result in higher percentage inhibition compared with that of the free enzyme. Copyright © 2008 Society of Chemical Industry