超高效液相色谱-串联质谱法测定鸡蛋中氯霉素的两种前处理方法比较
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摘要
为选择氯霉素超高效液相色谱串联质谱分析前处理方法,分别对乙酸乙酯提取,正己烷液液萃取净化和乙腈提取,LC-Si固相萃取柱萃取净化(GB/T22338-2008方法),两种前处理方法进行对比分析。结果显示:乙酸乙酯提取法的检测限为0.1μg/kg,在0.5～10 ng/mL范围内线性关系良好,r>0.99,回收率为98.2%～104.8%,RSD为1.5%～7.2%;乙腈提取法的检测限为0.05μg/kg,在0.25～10 ng/mL范围内线性关系良好,r>0.995,回收率为100.0%～104.0%%,RSD值为0.5%～2.1%。结果表明:两种方法的线性范围、回收率、检测限和相对偏差均能满足畜产品检验要求。乙酸乙酯提取法步骤简单,样品处理效率高,乙腈提取法虽步骤繁琐,但结果的精密度和灵敏度更高。
In order to select a method for the processing of chloramphenicol using ultra performance liquid chromatography-tandem mass spectrometry, two sample pre-processing methods for determination of chloramphenicol in eggs were compared in this study. One was ethyl acetate extraction with n-hexane purification, and the other was acetonitrile extraction with LC/Si solid phase extraction column purification(GB/T22338-2008). The results were as follows: The LOD of the ethyl acetate extraction method was 0.1 μg/kg, the calibration curve was admirably linear in the range of 0.5 to 10 ng/mL, R>0.99, the RSD of this method was 1.5%-7.2%, the recovery rate was 98.2%-104.8%. The LOD of the acetonitrile extraction method was 0.05 μg/kg, the calibration curve was admirably linear in the range of 0.25 to 10 ng/mL, R>0.995, the RSD of this method was 0.5%-2.1%, the recovery rate was 100.0%-104.0%. The above results indicated that the linear range, recovery rate, detection limit and relative deviation of the two methods could all meet the requirements for animal product inspection. The extraction method of ethyl acetate extraction was simpler and more efficient, while the acetonitrile extraction method was a little cumbersome, but was more precise and sensitive.
In order to select a method for the processing of chloramphenicol using ultra performance liquid chromatography-tandem mass spectrometry, two sample pre-processing methods for determination of chloramphenicol in eggs were compared in this study. One was ethyl acetate extraction with n-hexane purification, and the other was acetonitrile extraction with LC/Si solid phase extraction column purification(GB/T22338-2008). The results were as follows: The LOD of the ethyl acetate extraction method was 0.1 μg/kg, the calibration curve was admirably linear in the range of 0.5 to 10 ng/mL, R>0.99, the RSD of this method was 1.5%-7.2%, the recovery rate was 98.2%-104.8%. The LOD of the acetonitrile extraction method was 0.05 μg/kg, the calibration curve was admirably linear in the range of 0.25 to 10 ng/mL, R>0.995, the RSD of this method was 0.5%-2.1%, the recovery rate was 100.0%-104.0%. The above results indicated that the linear range, recovery rate, detection limit and relative deviation of the two methods could all meet the requirements for animal product inspection. The extraction method of ethyl acetate extraction was simpler and more efficient, while the acetonitrile extraction method was a little cumbersome, but was more precise and sensitive.
引文
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[6] 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、鸡蛋中氯霉素和甲硝唑残留[J].中国卫生检验杂志,2016,(21):3083-3085.
[7] 温家欣,吴凤丹,曹雅静,等.超高效液相色谱-串联质谱法测定蜂胶及以其为原料的保健食品中的氯霉素[J].色谱,2018,36(12):1284-1289.
[8] 曾勇,董文婷,龚波,等.超高效液相色谱-串联质谱法快速测定禽蛋中氯霉素、氟苯尼考及其代谢物残留[J].中国兽药杂志,2017,(12):42-46.
[2] 中华人民共和国农业部公告第235号[Z].北京:中华人民共和国农业部,2002.
[3] 鞠中杰,王倩倩.液相色谱串联质谱内标法测定猪肉中氯霉素的不确定度评定[J].现代食品,2019(06):149-153.
[4] GB/T22338-2008.动物源性食品中氯霉素类药物残留量测定[S].
[5] Lu L,Li J,Jin SH,et al.Combination of reversed phase liquid chromatography and zwitterion exchange reversed phase hydrophilic interaction mixed mode liquid chromatography coupled with mass spectrometry for the analysis of antibiotics and their impurities[J].J Chin Pharm Sci,2014,23(2):106-117.
[6] 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、鸡蛋中氯霉素和甲硝唑残留[J].中国卫生检验杂志,2016,(21):3083-3085.
[7] 温家欣,吴凤丹,曹雅静,等.超高效液相色谱-串联质谱法测定蜂胶及以其为原料的保健食品中的氯霉素[J].色谱,2018,36(12):1284-1289.
[8] 曾勇,董文婷,龚波,等.超高效液相色谱-串联质谱法快速测定禽蛋中氯霉素、氟苯尼考及其代谢物残留[J].中国兽药杂志,2017,(12):42-46.