新疆农业科学 ›› 2023, Vol. 60 ›› Issue (3): 683-688.DOI: 10.6048/j.issn.1001-4330.2023.03.019
• 植物保护·设施农业·农产品加工工程·微生物 • 上一篇 下一篇
田锋1,2(), 包东东2, 徐智明2, 杨婧2, 李娟2, 刘晓红2, 谭慧林2(), 张志东1,2()
收稿日期:
2022-08-20
出版日期:
2023-03-20
发布日期:
2023-04-18
通信作者:
谭慧林(1977-),女,新疆乌鲁木齐人,正高级工程师,研究方向为食品安全检验,(E-mail)45118707@qq.com;作者简介:
田锋(1990-),男,新疆阿克苏人,工程师,研究方向为食品安全检验,(E-mail)121745510@qq.com
基金资助:
TIAN Feng1,2(), BAO Dongdong2, XU Zhiming2, YANG Jing2, LI Juan2, LIU Xiaohong2, TAN Huilin2(), ZHANG Zhidong1,2()
Received:
2022-08-20
Online:
2023-03-20
Published:
2023-04-18
Correspondence author:
TAN Huilin(1977-),female,Native place:Urumqi, Xinjiang. Research Professor professial,research field: food safety inspection,(E-mail)Supported by:
摘要:
【目的】提高苹果中克百威残留快速检测方法的灵敏度与准确度,确保苹果产品中克百威农药残留抽查的高效和准确性。【方法】以新疆阿克苏当地6个点位市售苹果为检测样品,采用行业标准NY/T 761-2008第3部分的液相色谱法为参比方法,分别选择3家快检试剂盒,根据《食品快速检测方法评价技术规范》对其快检适应性进行评估。【结果】利用参比方法和快检试剂盒均未从苹果样品中检出克百威残留。3家快检试剂盒可在0.01 mg/kg以上呈阳性显色反应,低于GB/T 2763-2019《食品安全国家标准食品中农药最大残留限量》中的限量要求;试剂盒灵敏度均为100%、特异性均为50%、假阴性率均为0、假阳性率均为50%、相对准确度均为90%。【结论】所测试剂盒适用于苹果中克百威残留量的快速筛查。
中图分类号:
田锋, 包东东, 徐智明, 杨婧, 李娟, 刘晓红, 谭慧林, 张志东. 苹果中克百威残留快检测定及方法评估[J]. 新疆农业科学, 2023, 60(3): 683-688.
TIAN Feng, BAO Dongdong, XU Zhiming, YANG Jing, LI Juan, LIU Xiaohong, TAN Huilin, ZHANG Zhidong. Evaluation of Rapid Detection Method for Carbofuran Residues in Apples[J]. Xinjiang Agricultural Sciences, 2023, 60(3): 683-688.
样品情况a Samplea | 检测结果b Resultb | 总数 Total | |
---|---|---|---|
阳性 Positive | 阴性 Negative | ||
阳性Positive | N11 | N12 | N1.=N11+N12 |
阴性Negative | N21 | N22 | N2.=N21+N22 |
总数Tatol | N.1=N11+N21 | N.2=N12+N22 | N=N1.+N2.或N.1+N.2 |
显著性差异(x2)Significant difference (x2) | x2=( N12-N21 -1)2/(N12+N21),自由度(df)=1 | ||
灵敏度(p+,%)sensitivity (p+,%) | p+=N11/N1. | ||
特异性(p-,%)Specificity (p-,%) | p-=N22/N2. | ||
假阴性率(pf-,%)False negative rate (pf-,%) | pf-=N12/N1.=100-灵敏度 | ||
假阳性率(pf+,%)False positive rate (pf+,%) | pf+=N21/N2.=100-特异性 | ||
相对准确度,%cRelative accuracy %c | (N11+N22)/(N1.+N2.) |
表1 快速检测方法性能指标计算
Tab.1 The calculation of properties indexes of the rapid detection method
样品情况a Samplea | 检测结果b Resultb | 总数 Total | |
---|---|---|---|
阳性 Positive | 阴性 Negative | ||
阳性Positive | N11 | N12 | N1.=N11+N12 |
阴性Negative | N21 | N22 | N2.=N21+N22 |
总数Tatol | N.1=N11+N21 | N.2=N12+N22 | N=N1.+N2.或N.1+N.2 |
显著性差异(x2)Significant difference (x2) | x2=( N12-N21 -1)2/(N12+N21),自由度(df)=1 | ||
灵敏度(p+,%)sensitivity (p+,%) | p+=N11/N1. | ||
特异性(p-,%)Specificity (p-,%) | p-=N22/N2. | ||
假阴性率(pf-,%)False negative rate (pf-,%) | pf-=N12/N1.=100-灵敏度 | ||
假阳性率(pf+,%)False positive rate (pf+,%) | pf+=N21/N2.=100-特异性 | ||
相对准确度,%cRelative accuracy %c | (N11+N22)/(N1.+N2.) |
克百威 加标浓度 Concentration of carbofuran spiked level (mg/kg) | 检测值1 Test value (mg/kg) | 检测值2 Test value (mg/kg) | 检测值3 Test value (mg/kg) | 回收率 Rate of recovery (%) |
---|---|---|---|---|
0.1 | 0.087 | 0.084 | 0.082 | 82~87 |
0.2 | 0.183 | 0.186 | 0.180 | 90~93 |
0.4 | 0.379 | 0.389 | 0.384 | 94~97 |
0.8 | 0.769 | 0.805 | 0.772 | 96~101 |
1.0 | 0.960 | 0.945 | 0.981 | 94~98 |
表2 不同浓度克百威加标回收率
Tab.2 Recovery rate of carbofuran with different concentrations
克百威 加标浓度 Concentration of carbofuran spiked level (mg/kg) | 检测值1 Test value (mg/kg) | 检测值2 Test value (mg/kg) | 检测值3 Test value (mg/kg) | 回收率 Rate of recovery (%) |
---|---|---|---|---|
0.1 | 0.087 | 0.084 | 0.082 | 82~87 |
0.2 | 0.183 | 0.186 | 0.180 | 90~93 |
0.4 | 0.379 | 0.389 | 0.384 | 94~97 |
0.8 | 0.769 | 0.805 | 0.772 | 96~101 |
1.0 | 0.960 | 0.945 | 0.981 | 94~98 |
项目 Sample | 试剂盒1 No.1 Kit | 试剂盒2 No.2 Kit | 试剂盒3 No.3 Kit | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
阴性 Postive | 阳性 Negative | 阴性 Postive | 阳性 Negative | 阴性 Postive | 阳性 Negative | ||||||||
克百威 加标浓度 Concentration of carbofuran spiked level (mg/kg) | 0 | 50 | 0 | 50 | 0 | 50 | 0 | ||||||
0.01 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.02 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.05 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.1 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.2 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.5 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
1.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
2.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
5.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
灵敏度Sensitivity(%) | 100 | 100 | 100 | ||||||||||
特异性Specificity(%) | 50 | 50 | 50 | ||||||||||
假阳性率False positive rate(%) | 50 | 50 | 50 | ||||||||||
假阴性率False negative rate(%) | 0 | 0 | 0 | ||||||||||
相对准确度Relative accuracy(%) | 90 | 90 | 90 | ||||||||||
显著性差异Significant difference | 52.02 | 52.02 | 52.02 |
表3 不同克百威加标浓度快检结果
Tab.3 Rapid detection results of carbofuran with different spiked concentrations
项目 Sample | 试剂盒1 No.1 Kit | 试剂盒2 No.2 Kit | 试剂盒3 No.3 Kit | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
阴性 Postive | 阳性 Negative | 阴性 Postive | 阳性 Negative | 阴性 Postive | 阳性 Negative | ||||||||
克百威 加标浓度 Concentration of carbofuran spiked level (mg/kg) | 0 | 50 | 0 | 50 | 0 | 50 | 0 | ||||||
0.01 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.02 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.05 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.1 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.2 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
0.5 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
1.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
2.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
5.0 | 0 | 50 | 0 | 50 | 0 | 50 | |||||||
灵敏度Sensitivity(%) | 100 | 100 | 100 | ||||||||||
特异性Specificity(%) | 50 | 50 | 50 | ||||||||||
假阳性率False positive rate(%) | 50 | 50 | 50 | ||||||||||
假阴性率False negative rate(%) | 0 | 0 | 0 | ||||||||||
相对准确度Relative accuracy(%) | 90 | 90 | 90 | ||||||||||
显著性差异Significant difference | 52.02 | 52.02 | 52.02 |
[1] | Yang J Y, Zhang Y, Wang H, et al. Development of fluorescence polarisation immunoassay for carbofuran in food and environmental water samples[J]. Food & Agricultural Immunology, 2014, 26(3):340-355. |
[2] | 陈建波, 王云飞, 奚道珍. 克百威及其代谢产物残留分析方法研究进展[J]. 农药科学与管理, 2011, 32(3):30-33. |
CHEN Jianbo, WANG Yunfei, XI Daozhen. Review of methods for determination of carbofuran and its metabolites[J]. Pesticide Science and Administration, 2011, 32(3):30-33. | |
[3] | 中国农业工业协会. 2016年国家禁用和限用的农药名录汇总[J]. 今日农药, 2017,(2):9. |
China Agricultural Industry Association. Summary of the list of pesticides banned and restricted by the state in 2016[J]. The New Century of Agrochem, 2017,(2):9. | |
[4] | 徐广洲, 何苗. 盐城市售蔬菜农药残留状况调查和风险评估[J]. 科技创新导报, 2017, 14(36):114-116. |
XU Guangzhou, HE Miao. Investigation and risk assessment of pesticide residues in vegetables sold in Yancheng[J]. Science and Technology Innovation Guide, 2017, 14(36):114-116. | |
[5] | 徐静, 代飞飞, 聂丹丹. 潍坊市2015年蔬菜、水果中农药残留污染情况[J]. 中国热带医学, 2016, 16(2):141-144, 148. |
XU Jing, DAI FeiFei, NIE Dandan. Situation of pesticide residues in vegetables and fruits of Weifang City in 2015[J]. China Tropical Medicine, 2016, 16(2):141-144,148. | |
[6] | 郑庆伟. 内蒙古:尖椒克百威超标都是假药60%菌虫双杀烟剂惹的祸[J]. 农药市场信息, 2018, 612(3):17. |
ZHENG Qingwei. Inner Mongolia: The over standard of carbofuran in jianjiao is caused by the fake pesticide[J]. Pesticide Market News, 2018, 612(3):17. | |
[7] | 谭慧林, 金永生, 吴忠红, 等. 阿克苏地区红富士苹果产业现状及提高商品性建议措施[J]. 保鲜与加工, 2021, 21(2):140-144. |
TAN Huilin, JIN Yongsheng, WU Zhonghong, et al. Status of Red Fuji Apple Industry in Aksu Prefecture and Measures to Improve Its Commodity Quality[J]. Storage and Process, 2021, 21(2):140-144. | |
[8] | 韦林洪, 刘曙照, 邵秀金. 免疫亲和色谱-高效液相色谱法测定河水和土壤中克百威、三唑磷和绿磺隆残留量[J]. 理化检验(化学分册), 2012, 48(8):887-892. |
WEI Linhong, LIU Shuzhao, SHAO Xiujin. IAC-HPLC Determination of Residual Amounts of Carbofuran, Triaophos and Chlorsulfuran in River Water and Soil[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2012, 48(8):887-892. | |
[9] | 高强, 孙榕, 高升成, 杨治彪, 等. 高效液相色谱-柱后衍生法测定蔬菜中克百威农药残留量的不确定度评定[J]. 现代农业科技, 2019(19):101-102,107. |
GAO Qiang, SUN Rong, GAO Shengcheng, et al. Evaluation of Uncertainty in Determination of Carbofuran Pesticide Residues in Vegetables by High Performance Liquid Chromatography-Post-Column Derivatization[J]. Modern Agricultural Science and Technology, 2019(19):101-102,107. | |
[10] | 连翠飞, 田景升, 郭孝辉, 等. QuEChERS-高效液相色谱法测定食品中4种氨基甲酸酯类农药残留[J]. 中国酿造, 2020, 39(8):206-209. |
LIAN Cuifei, TIAN Jingsheng, GUO Xiaohui, et al. Determination of four kinds of carbamate pesticide residues in food by QuEChERS-HPLC[J]. China Brewing, 2020, 39(8):206-209. | |
[11] | 孙盈盈. 气相色谱法检测水产品中呋喃丹的残留[D]. 武汉: 华中农业大学, 2013. |
SUN Yingying. Determination of Carbofuran in Aquatic Products by Gas Chromatography[D]. Wuhan: Huazhong Agriculture University, 2013. | |
[12] | 杜启东, 梁耀娟. 气相色谱法在水产品中呋喃丹残留的检测研究[J]. 食品安全导刊, 2016,(12):106. |
DU Qidong, LIANG Yaojuan. Determination of carbofuran residues in aquatic products by gas chromatography[J]. China Food Safety Magazine, 2016,(12):106. | |
[13] | 韩璐, 黄大波. 气相色谱-质谱法快速测定葡萄中克百威残留量[J]. 现代农药, 2017, 16(3):38-39,44. |
HAN Lu, HUANG Dabo. Rapid Determination of Carbofuran Residue in Grape by GC-MS[J]. Modern Agrochemicals, 2017, 16(3):38-39,44. | |
[14] | 褚能明, 杨俊英, 李典晏, 等. 气相色谱-串联质谱法测定露地芹菜中丁硫克百威及其代谢物残留[J]. 南方农业学报, 2019, 50(8):1822-1828. |
CHU Nengming, YANG Junying, LI Dianyan, et al. Determination of carbosulfan and its metabolitesin field celery by gas chromatography-tandem mass spectrometry[J]. Southern Agriculture, 2019, 50(8):1822-1828. | |
[15] | 张振山, 乐渊, 黎舒怀, 等. QuEChERS-超高效液相色谱-串联质谱法检测中药砂仁中10种氨基甲酸酯类农药残留[J]. 安徽农业科学, 2021, 49(1):199-202,206. |
ZHANG Zhengshan, LE Yuan, LI Suhuai, et al. Determination of 10 Carbamate Pesticide Residues in Amomum villosum Lour. by QuEChERS-Ultra Performance Liquid Chroma-tography-Tandem Mass Spectrometry[J]. Journal of Anhui Agricultural Sciences, 2021, 49(1):199-202,206. | |
[16] | 李顺红. 超高效液相色谱-串联质谱法快速检测芹菜中农药残留[J]. 现代食品, 2020,(2):218-220. |
LI Shunhong. Rapid Detection by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry Pesticide Residues in Celery[J]. Modern Food, 2020,(2):218-220. | |
[17] | 韩吉祥. 液相色谱-质谱法对蔬菜水果中农药残留克百威进行检测的方法探讨[J]. 食品界, 2020,(10):126-127. |
HAN Jixiang. Determination of Carbofuran Residues in Vegetables and Fruits by LC-MS Spectrometry[J]. Food Industry, 2020,(10):126-127. | |
[18] | 王金艳. 食品快检技术在基层食品安全监管中的应用分析[J]. 食品安全导报, 2018, 11(15):84. |
WANG Jinyan. Analysis on the application of fast food inspection technology in grass-roots food safety supervision[J]. China Food Safety Magazine, 2018, 11(15):84. | |
[19] | 朱星晔, 杨志宾, 刘海玲. 基层食品快检中存在的问题和对策探讨[J]. 食品安全导报, 2018, 11(9):116. |
ZHU Xingye, YANG Zhibing, LIU Hailin. Discussion on the problems and Countermeasures in the quick inspection of basic food[J]. China Food Safety Magazine, 2018, 11(9):116. | |
[20] | 林伟琦. 食品安全快速检测技术的应用研究进展[J]. 食品安全质量检测学报, 2020, 11(3):961-967. |
LIN Weiqi. Research progress on application of rapid food safety detection technology[J]. Journal of Food Safety and Quality, 2020, 11(3):961-967. | |
[21] | 国家食品药品监督管理局. 食药监办科[2017]43号总局办公厅关于印发食品快速检测方法评价技术规范的通知[EB/OL].(2017-03-31)[2019-07-14]. http://samr.cfda.gov.cn/WS01/CL1605/171311.html. |
China Food, and Drug Administration. Food and Drug Administra-tion branch [2017]General Office 43 about Circular on printing and distributing evaluation the technical specifications for food safety rapid detection.[EB/OL].(2017-03-31)[2019-07-14]. http://samr.cfda.gov.cn/WS01/CL1605/171311.html. | |
[22] | NY/T 761-2003. 蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S]. |
NY/T 761-2003. Pesticide multiresidue screen methods for determination of organophosphorus pesticides, organochlorine pesticides, pyrethroid pesticides and carbamate pesticedes in vegetables and fruits[S]. | |
[23] | GB/T 27404-2008. 实验室质量控制规范食品理化检测[S]. |
GB/T 27404-2008. Criterion on Quality Control of Laboratories-Molecular Biological Testing of Food[S]. | |
[24] |
Liu L, Luo L, Suryoprabowo S, et al. Development of an immunochromatographic strip test for rapid detection of ciprofloxacin in milk samples[J]. Sensors, 2014, 14(9):16785-16798.
DOI PMID |
[25] | 岳清洪, 黄瑛, 黄璐瑶, 等. 食品安全快速检测技术基层监管中存在的问题及对策[J]. 食品安全质量检测学报, 2019, 10(18):6356-6361. |
YUE Qinghong, HUANG Ying, HUANG Luyao, et al. Problems and countermeasures in the grassroots supervision of food safety fast detection technology[J]. Journal of Food Safety and Quality, 2019, 10(18):6356-6361. | |
[26] | 蔡新发, 张帆, 张家赫, 等. 氟喹诺酮类药物免疫分析方法研究进展[J]. 现代农业科技, 2018(9):266-267,272. |
CAI Xinfa, ZHANG Fan, ZHANG Jiahe, et al. Research progress on Immunoassay for Determunation of Fluoroquinolones[J]. Modern Agricultural Science and Technology, 2018(9):266-267,272. | |
[27] |
Guo S, Zhang W, He L, et al. Rapid evaluation of artesunate quality with a specific monoclonal antibody-based lateral flow dipstick[J]. Analytical and Bioanalytical Chemistry, 2016, 408(22):6003-6008.
DOI PMID |
[1] | 程功, 李悦, 刘立强, 尤璐瑶, 曼苏尔·那斯尔, 廖康. 新源野果林3种野生果树春播成苗特性分析[J]. 新疆农业科学, 2023, 60(7): 1722-1730. |
[2] | 孙小惠, 李静, 玛尔哈巴·帕尔哈提, 王贤, 马玉娥, 汪晖, 朱靖蓉. 不同等级阿克苏冰糖心苹果在低温贮藏条件下营养成分变化[J]. 新疆农业科学, 2023, 60(5): 1181-1189. |
[3] | 李静霞, 张学祥, 李丰, 马思洁, 张萍, 朱天生. 基于MaxEnt模型的柳树植原体病害在我国的适生区预测及定量风险分析[J]. 新疆农业科学, 2023, 60(5): 1235-1243. |
[4] | 封帆, 谢开云, 艾比布拉·伊马木, 万江春. 果园生草对苹果园杂草控制、土壤养分及果树营养状况的影响[J]. 新疆农业科学, 2023, 60(4): 982-991. |
[5] | 王迎超, 张婧婧, 达新民, 耿新雪. 基于K-means与KNN的多特征苹果在线分级[J]. 新疆农业科学, 2023, 60(3): 643-650. |
[6] | 王凯, 李秀玲, 白茹, 冯建荣, 杨伟伟. 富士和嘎啦苹果叶片面积估算模型构建[J]. 新疆农业科学, 2023, 60(3): 664-674. |
[7] | 冯贝贝, 梅闯, 王磊, 耿文娟, 阿孜古丽·衣该木, 闫鹏, 王继勋. 阿克苏富士苹果烟富3号化学疏花疏果的效果[J]. 新疆农业科学, 2023, 60(10): 2470-2478. |
[8] | 李春艳, 刘芳婷, 张王斌. 基于高通量测序对引起苹果外观异常病原的鉴定[J]. 新疆农业科学, 2023, 60(1): 171-177. |
[9] | 兖攀, 王久照, 姜继元, 陈奇凌. 不同地面覆盖材料对绿洲苹果园土壤环境的影响[J]. 新疆农业科学, 2022, 59(7): 1690-1696. |
[10] | 曹辉, 王洪博, 张楠, 王兴鹏. 矮砧密植苹果光合特性及产量对水分的响应[J]. 新疆农业科学, 2022, 59(6): 1409-1417. |
[11] | 周晓明, 张付春, 钟海霞, 张雯, 韩守安, 伍新宇, 潘明启. 厂形叶幕赤霞珠葡萄果实苹果酸的代谢规律[J]. 新疆农业科学, 2022, 59(4): 855-862. |
[12] | 李晓磊, 王克众, 潘俨, 马燕, 徐斌, 张平, 孟新涛. 非浓缩还原苹果汁加工过程中物料感官品质的变化[J]. 新疆农业科学, 2022, 59(3): 645-656. |
[13] | 秦欢, 乔力潘·也森太, 塔马夏·吾拉力别克, 孙惠敏, 冯丽凯, 王少山. 不同防治措施下2种诱捕器对苹果蠹蛾田间诱集效果比较[J]. 新疆农业科学, 2022, 59(3): 683-690. |
[14] | 李亚鹏, 张王斌, 仪子博. 苹果树腐烂病病原种类及其亲缘关系分析[J]. 新疆农业科学, 2022, 59(3): 700-706. |
[15] | 谭慧林, 吴忠红, 金永生, 牛贵洋, 包东东, 陈海元, 张志东. 食品中金黄色葡萄球菌的快速检测及其评估[J]. 新疆农业科学, 2022, 59(2): 410-416. |
阅读次数 | ||||||
全文 |
|
|||||
摘要 |
|
|||||