超高效液相色谱-串联质谱法测定猪肉和鱼肉中氯霉素残留
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摘要
目的建立猪肉和鱼肉中氯霉素残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法以氘代氯霉素为内标,用含0.2%甲酸乙腈-水(80:20)提取样品中的氯霉素, Oasis PRiME HLB柱净化,采用BEH C_(18)(2.1 mm×100 mm,1.7μm)柱分离,柱温为30℃,以乙腈-0.1%甲酸的水溶液为流动相,梯度洗脱,流速为0.25 ml/min;质谱检测,ESI~-模式。结果方法线性范围为0.1μg/L～10μg/L,目标物在测定的浓度范围内,线性关系良好,相关系数>0.999 9,检出限为0.012μg/kg;用3种浓度做加标回收,回收率为83.2%～91.2%,相对标准偏差为2.94%～6.26%。结论本法快速、灵敏,操作简便,检测结果准确度高,能满足日常猪肉和鱼肉样品中的氯霉素残留的检测要求。
Objective To establish a method for the determination of chloramphenicol residues in pork and fish with liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Using deuterated chloramphenicol as the internal standard, chloramphenicol was extracted from the sample using 0.2% acetonitrile formate-water(80:20, V/V), then purified with Oasis PRiME HLB column, and finally separated with BEH C_(18)(2.1 mm×100 mm, 1.7 μm) column when temperature was 30 ℃. Acetonitrile-0.1% formic acid aqueous solution was used as a mobile phase for gradient elution with the flow rate 0.25 ml/min. The detection was performed by using mass spectrometer and ESI~- mode. Results The linear range was within 0.1 μg/L-10 μg/L, and the target had a good linear relationship in the determined concentration range, with the correlation coefficient greater than 0.999 9. The detection limit was set as 0.012 μg/kg. Three concentrations were used for standard recovery, which was within 83.2%-91.2%, and the relative standard deviation was within 2.94%-6.26%. Conclusion This method is quick, sensitive, easy-operate, and accurate. It can be applied to the determination of chloramphenicol residue in daily pork and fish samples.
Objective To establish a method for the determination of chloramphenicol residues in pork and fish with liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Using deuterated chloramphenicol as the internal standard, chloramphenicol was extracted from the sample using 0.2% acetonitrile formate-water(80:20, V/V), then purified with Oasis PRiME HLB column, and finally separated with BEH C_(18)(2.1 mm×100 mm, 1.7 μm) column when temperature was 30 ℃. Acetonitrile-0.1% formic acid aqueous solution was used as a mobile phase for gradient elution with the flow rate 0.25 ml/min. The detection was performed by using mass spectrometer and ESI~- mode. Results The linear range was within 0.1 μg/L-10 μg/L, and the target had a good linear relationship in the determined concentration range, with the correlation coefficient greater than 0.999 9. The detection limit was set as 0.012 μg/kg. Three concentrations were used for standard recovery, which was within 83.2%-91.2%, and the relative standard deviation was within 2.94%-6.26%. Conclusion This method is quick, sensitive, easy-operate, and accurate. It can be applied to the determination of chloramphenicol residue in daily pork and fish samples.
引文
[1] 文卫,钮伟民,许伟芳.氯霉素残留检验技术的研究进展[J].现代预防医学,2007,34(1):67-68.
[2] 曹巧玲,杨凯,武泽新.氯霉素的毒性作用和检测方法研究进展[J].职业与健康,2013,29(16):2095-2097.
[3] 张凤清,王岩松,范世华,等.高效液相色谱法测定动物肌肉组织中的氯霉素,甲砜霉素和氟苯尼考残留量[J].食品科学,2010,8(31):248-251.
[4] 占春瑞,郭平,陈振桂,等.超高效液相色谱法测定水产品中甲砜霉素和氟甲砜霉素残留[J].分析化学,2008,36(4):525-528.
[5] 杨黎,廖夏云,杨伟婷,等.高效液相色谱法-串联质谱法测定以蜂胶为主要原料的保健食品中的氯霉素[J].食品科学,2016,37(16):263-267.
[6] 洪振涛,张卫峰,聂建荣,等.气相色谱法测定动物组织氯霉素的残留量[J].中国兽药杂志,2006,40(2):14-15.
[7] 李应国,赵旭博,张雷,等.免疫亲和柱-高效液相色谱法检测乳制品中氯霉素[J].中国乳品工业,2011,39(4):53-54.
[8] 蒋定国.高效液相色谱法测牛奶中氯霉素残留量的研究[J].中国食品卫生杂志,2003,15(1):36-38.
[9] 国家质量监督检验检疫总局.GB/T 22338—2008 动物源性食品中氯霉素类药物残留量测定[S].北京:中国标准出版社,2008.
[10] 刘跃坤,刘崇奇.对GB/T 22338—2008 气相色谱质谱联用仪负化学源检测食品中氯霉素残留量方法的改进与补充[J].食品安全质量检测学报,2016,7(1):74-78.
[11] 李海平,张树海,张坤生.GC-MS分析法在猪肉氯霉素残留检测中的应用[J].食品与机械,2006,22(5):89-92.
[12] 魏林阳,徐金晶,吴红军.水厂品中氯霉素残留的气质联用法检测[J].光谱实验室,2007,24(2):201-205.
[13] 胡争艳,吴平谷,王天娇,等.超高效液相色谱-串联质谱法同时测定鸡肉鸡蛋中胡氯霉素和甲硝唑残留[J].中国卫生检验杂志,2016,36(21):3083-3085.
[14] 陈剑刚,张艳,白艳玲,等.同位素内标稀释液相色谱-串联质谱测定虾中氯霉素、甲砜霉素、氟甲砜霉素残留量[J].中国卫生检验杂志,2013,23(7):1670-1673.
[15] 蔡欣欣,张秀尧.超高效液相色谱三重四级杆质谱法快速测定动物源食品中的氯霉素、甲砜霉素、氟苯尼考残留[J].中国卫生检验杂志,2009,19(2):258-260.
[2] 曹巧玲,杨凯,武泽新.氯霉素的毒性作用和检测方法研究进展[J].职业与健康,2013,29(16):2095-2097.
[3] 张凤清,王岩松,范世华,等.高效液相色谱法测定动物肌肉组织中的氯霉素,甲砜霉素和氟苯尼考残留量[J].食品科学,2010,8(31):248-251.
[4] 占春瑞,郭平,陈振桂,等.超高效液相色谱法测定水产品中甲砜霉素和氟甲砜霉素残留[J].分析化学,2008,36(4):525-528.
[5] 杨黎,廖夏云,杨伟婷,等.高效液相色谱法-串联质谱法测定以蜂胶为主要原料的保健食品中的氯霉素[J].食品科学,2016,37(16):263-267.
[6] 洪振涛,张卫峰,聂建荣,等.气相色谱法测定动物组织氯霉素的残留量[J].中国兽药杂志,2006,40(2):14-15.
[7] 李应国,赵旭博,张雷,等.免疫亲和柱-高效液相色谱法检测乳制品中氯霉素[J].中国乳品工业,2011,39(4):53-54.
[8] 蒋定国.高效液相色谱法测牛奶中氯霉素残留量的研究[J].中国食品卫生杂志,2003,15(1):36-38.
[9] 国家质量监督检验检疫总局.GB/T 22338—2008 动物源性食品中氯霉素类药物残留量测定[S].北京:中国标准出版社,2008.
[10] 刘跃坤,刘崇奇.对GB/T 22338—2008 气相色谱质谱联用仪负化学源检测食品中氯霉素残留量方法的改进与补充[J].食品安全质量检测学报,2016,7(1):74-78.
[11] 李海平,张树海,张坤生.GC-MS分析法在猪肉氯霉素残留检测中的应用[J].食品与机械,2006,22(5):89-92.
[12] 魏林阳,徐金晶,吴红军.水厂品中氯霉素残留的气质联用法检测[J].光谱实验室,2007,24(2):201-205.
[13] 胡争艳,吴平谷,王天娇,等.超高效液相色谱-串联质谱法同时测定鸡肉鸡蛋中胡氯霉素和甲硝唑残留[J].中国卫生检验杂志,2016,36(21):3083-3085.
[14] 陈剑刚,张艳,白艳玲,等.同位素内标稀释液相色谱-串联质谱测定虾中氯霉素、甲砜霉素、氟甲砜霉素残留量[J].中国卫生检验杂志,2013,23(7):1670-1673.
[15] 蔡欣欣,张秀尧.超高效液相色谱三重四级杆质谱法快速测定动物源食品中的氯霉素、甲砜霉素、氟苯尼考残留[J].中国卫生检验杂志,2009,19(2):258-260.
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