<4D F736F F D D BBAA2020BEEA2D2D2D2D2DB2CEBFBCCEC4CFD73133D3D0B5D7C9ABA3ACC7EBC8A5B3FD2E646F63>

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1 4 1 Vol. 4 No Journal of Food Safety and Quality Feb., 213 华 娟 1,2, 方勤美 3, 熊春娥 4, 吴少明 5, 陈立松 5, 郑奎城 1, 傅武胜 1,4,5* (1.,, 351; 2., 352; 3., 353; 4., 351; 5., 358) 摘要 : 目的 方法,,, / (LC-MC/MS), 结果 (.3μg/kg ), 31 %(71/229), 9.%(22/229) 1.31%(3/229),, (%, 3/3), (82.1%, 23/28) (75. %, 24/32) (4.7%, 7/15) (1.%, 12/75) (5.%, 2/3),, 结论, 关键词 : ; ; ; ; Survey of chloramphenicol residues in animal-origin foods in the retailer HUA Juan 1,2, FANG Qin-Mei 3, XIONG Chun- E 4, WU Shao-Ming 5, CHEN Li-Song 5, ZHENG Kui-Cheng 1, FU Wu-Sheng 1,4,5* (1. Fujian Provincial Key Laboratory of Zoonosis, Center for Disease Control and Prevention, Fuzhou 351, China; 2. College of Crop Science, Fujian Agriculture and Forestry University, Fuzhou 352, China; 3.Biotechnology Research Institute, Fujian Academy of Agricultural Sciences, Fuzhou 353, China; 4. College of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 351, China; 5. Key Laboratory of Analysis & Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 358, China) ABSTRACT: Objective To investigate the chloramphenicols residues of animal-original foods. Methods The edible portion of fish, shrimp and pork were ground with solidified carbon dioxide, homogenized and then stored in the frozen. The homogenized samples were extracted with ethyl acetate or acetonitrile, degreased with hexane, detected by liquid chromatography tandem mass spectrometry (LC-MS/MS), and quantified by internal standard method. Results The results obtained from the 229 samples showed that the positive rates of chloramphenicol florfenicol and thiamphenicol were 31.% (71/229) (according to detection limit.3 μg/kg), 9.% (22/229) and 1.31% (3/229), respectively. The detection rates of chloramphenicol were obviously dif- 基金项目 : (229) Fund: Supported by the National Health Welfare Industry-specific Foundation of China (229) * 通讯作者 :,,, fwsfqm@12.com *Corresponding author: FU Wu-Sheng, Chief Technician, Fujian Center for Disease Control and Prevention, No.7, Jintai Road, Gulou District, Fuzhou 351, China. fwsfqm@12.com

2 1 4 ferent among the samples. The relative higher detection rate was found in pollen(%, 3/3), followed by aquaculture fish (82.1%, 23/28), milk (75.%, 24/32), pork (4.7%, 7/15), domestic honey (1.%, 12/75) and imported honey (2/3, 5.%) except none of chloamphenicols detected in shrimps. Thiamphenicol were detected in pork, milk, fish but florfenicol were only detected in honey and pork, and their residual levels were below the tolerance. Conclusion The problem of chloramphenicol illegally used in the aquaculture and animal breeding still existed and the risk monitoring and legal action should be further strengthened. KEY WORDS: animal-original foods; chloramphenicol; thiamphenicol; florfenicol; residues survey 1 引言 [1],, (CAP) [2,3] 19 5 [4],, [5,] CAP, FAO/WHO (JECFA) 1994 CAP, 2 CAP, CPA, [7],, CAP, 22 CAP [8], [9], CAP 5% ; CAP.31 µg/kg, 5.2% [] ; CAP 17.%~ 3.% [11] (ELISA) [8,9] (HPLC) [11], ELISA (LC-MS/MS) [] ELISA HPLC,, LC/MS/MS,, (UPLC/MS/MS),,, 2 材料与方法 2.1 仪器与设备 ACQUITY ( Waters ); API 5 ( AB Sciex ); DFY-8 ( ); Microfuge Lite ( Beckman ); JZ-Ⅱ ( ); ( IKA ); G-5E ( Scientific Industries ); ( EYELA ); YP22N ( ); DPW N ( ); KQ-5B ( ); (DHG-9123A, ) 2.2 试剂与材料 试剂 ( 99.%, Sigma ); ( -D 5 )( 99.9%, Cambridge Isotope Laboratories );, Fisher 样品的采集 3 2,,,, 样品预处理 4 h,, 4~5,,,, 2~3 h,

3 1, : 17, 氯霉素类药物的检测方法 GB/T /,,, LC/MS/MS LC-MS/MS 测定条件 : Symmetry C 18 (Waters, 15 mm 39 mm, 5 μm); : 4 ;, A.1%, B ; : ml/min; : 5. µl 1 : (ESI) ; : ; : (MRM); : 45 V; : : : m/z321./151.7( ) 32.9/151.7( ); : m/z354./184.7( ) 354./289.( ); : m/z 35./335.7( ) 35./ 184.7( ), /min Initial 表 1 HPLC 流动相梯度洗脱条件 Table 1 Mobile phase gradient elution conditions for HPLC ml/min %A %B Curve 样品的制备与测定 4 : 5 g(.1 g) 5 ml, 2 μl d 5 -CAP (.1 ng/ml) 5 ml, 3 s, 5 min 35 ml, 5 min,, 4.5 ml,, 5 ml,.5 ml,,, 1.5 ml, 1 min,,, 2 ml, r/min 5 min, 2. ml,,, LC-MS/MS : 5 g(.1 g) 5 ml, 2 μl d 5 -CAP (.1 ng/ml) ml, 3 s, 5 min, 15 ml, 5 min, (, 85 r/min, 5 min),, 方法学指标的验证, CAP.3~.1 μg/kg,.1~.3 μg/kg, (.1 μg/kg).1~ ng/ml (r>.99).5 μg/kg, 73.7%~5%(n=), RSD 3.1%~13% 3 结果与分析 3.1 氯霉素 229, 31. %, 23.5 μg/kg, 9.%, 31.% 7,, CAP, 11.1 μg/kg,, CAP 82.1%, CAP (4.7%~75. %)( 2) 3,, 4%, 2.7% 3.2 氟甲砜霉素 (9. %)( 3), ( μg/kg) [2,3], 1 (38.4 μg/kg) 143

4 μg/kg,,, 3.3 甲砜霉素 229,, 1.31%, CAP,, ND~33.1 μg/kg ( 4), ( μg/kg) Table 2 ( ) ( ) 表 2 七类食品中氯霉素的检出率和残留量 Detection rate and residues of chloramphenicol in seven kinds of food (%) (μg/kg) (μg/kg) ~ ~ ( ) ~ ( ) ~ ~ ~ N.D. N.D.~ : N.D. (.3 μg/kg), (N.D.), μg/kg, Table 3 ( ) ( ) 表 3 七类食品中氟甲砜霉素的检出率和残留量 Detection rate and residues of florfenicol in seven kinds of food (%) (μg/kg) (μg/kg) 75 N.D ~ ~ ~ N.D. 3 N.D. 4 N.D N.D.~ : N.D. (.2 μg/kg) Table 4 ( ) ( ) 表 4 七类食品中甲砜霉素的检出率和残留量 Detection rate and residues of thiamphenicol in seven kinds of food (%) (μg/kg) (μg/kg) 3 N.D. 3 N.D N.D.~ N.D. 28 N.D N.D.~ N.D. N.D.~33.1 N.D.~.12 : N.D. (.5 μg/kg)

5 1, : 19 4 讨论 4.1 检出限对食品氯霉素检出率判定的影响, CAP (.3 μg/kg) GB/T (.1 μg/kg) 1/3, (.1 μg/kg) CAP, CAP 11.4%(2/229), CAP, CAP 4.7% 2.7%, CAP 82.1% 1.1% 21.4% 12.%, CAP 75%.3% CAP ( ), 4.2 水产品氯霉素药物残留问题 CAP, CAP,,, 354 ( ) CAP [15], CAP CAP [1], (4/4) CAP, CAP 41.9%, 1.82~4.5 μg/kg ; ( )CAP ~14.8%,.3 μg/kg, CAP (82.1%), CAP 4.3 蜂蜜和花粉中氯霉素残留, 75, 3,,, CAP CAP (1.1 ) (5.%), 25 (3/3, %) [1] 3 CAP,,, CAP, 4.4 牛奶和猪肉中氯霉素残留, (32 ), (75. %), [9],,, CAP, [9],, (HACCP),, CAP, CAP CAP 4.7%,, 参考文献 [1],. [J]., 22, 14(2): Jiang DG, Yang DJ. Detecting technology overview of chloramphenicol residue in animal food [J]. Chin J Food Hyg, 22, 14(2): [2] Stuart JA, Katharina H, Richard JF. Study of the distribution and depletion of chloramphenicol residues in bee products extracted from treated honeybee (Apis mellifera L.) [J]. Biomed Life Sci, 28, 39(5): [3] Holt D, Harvey D, Hurley R. Chloramphenicol toxicity [J]. Adverse Drug React Toxicol Rev, 1993, 12(2): [4] Reinhard Z, Hakan E, Heinz S. Assessment of commutability for candidate certified reference material ERM-BB13 chloramphenicol in pork [J]. Anal Bioanal Chem, 2, 398(3): [5],,,. [J]., 24, 31(1): Hou WD, Fu XL, Yang Y, et al. Level of veterinary drug residues in animal food and dietary safety evaluation [J]. Mod Prevent Med, 24, 31(1): [],. [J]., 21, 35(5): Hu DF, Shen JZ. Chloramphenicol antibiotic residue analysis [J]. Chin J Vet Drug, 21, 35(5): [7] Takino M, Daishima S, Nakahara T. Determination of chloramphenicol residues in fish meats by liquid chromatography-atmospheric pressure photoionization mass spectrometry [J]. J Chromatogr A, 23, 11(1): [8]. [J]., 211, (): 3 5. Cui HH. The investigation and detection analysis of chloramphenicol, tetracycline antibiotic residues of fresh and sterilization milk in parts of Zhejiang [J]. Guangxi J Light ind, 211, (): 3 5.

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