悬浮固化液相微萃取-高效液相色谱联用测定水样中甲硝唑和氯霉素
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摘要
建立了悬浮固化液相微萃取-高效液相色谱法同时测定水样中甲硝唑和氯霉素的分析方法。采用正交实验设计对萃取多因素进行考查,如萃取剂的种类及用量、萃取温度、NaCl浓度、pH值和搅拌速度等进行优化,在最佳萃取条件下,甲硝唑和氯霉素浓度在10～400μg/mL范围内具有良好线形关系,线形相关系数分别为0.995和0.997,检出限分别为0.48μg/mL和0.98μg/mL(S/N=3),加标回收率在79.5～82.9%。方法简便、准确、专属性强,可用于测定水样中甲硝唑和氯霉素。
Important experimental parameters affecting the extraction process were optimized by orthogonal experimental design.The type and usage of extraction solvent,extraction temperature,concentration of NaCl,pH value and stirring rate were investigated.Under the optimum conditions,agood linearity was in the concentration range of 10—400μg/mL for metronidazole and chloroamphenicol.The correlation correlation coefficients(r)were 0.995 and 0.997,respectively,the limits of detection were 0.48μg/mL and 0.98μg/mL(S/N=3),respectively.The recoveries were in the range of 79.5% and 82.9%.The method is simple,sensitive and accurate,can be used for the determination of metronidazole and chloroamphenicol in water samples.
Important experimental parameters affecting the extraction process were optimized by orthogonal experimental design.The type and usage of extraction solvent,extraction temperature,concentration of NaCl,pH value and stirring rate were investigated.Under the optimum conditions,agood linearity was in the concentration range of 10—400μg/mL for metronidazole and chloroamphenicol.The correlation correlation coefficients(r)were 0.995 and 0.997,respectively,the limits of detection were 0.48μg/mL and 0.98μg/mL(S/N=3),respectively.The recoveries were in the range of 79.5% and 82.9%.The method is simple,sensitive and accurate,can be used for the determination of metronidazole and chloroamphenicol in water samples.
引文
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[12]卢巧梅,张文敏,黄川辉,等.悬浮固化液相微萃取-高效液相色谱法分析生长素[J].福州大学学报(自然科学版),2015,43(4):554-559.
[2]汪梦蝶.甲硝唑片的质量一致性评价研究[D].武汉:华中科技大学,2018.
[3]胡顶飞,沈建忠.氯霉素类抗生素残留分析[J].中国兽药杂志,2001,35(5):55-57.
[4]罗文婷,吴青,简伟明,等.超高效液相色谱法测定水产品中违禁兽药氯霉素、呋喃唑酮和甲硝唑残留[J].分析化学,2009,37(6):877-880.
[5]倪晓丹.碳纳米管固相萃取检测环境样品中痕量抗生素及农药的残留[D].广州:华南师范大学,2011.
[6]刘伟,张楠,李兵,等.固相萃取-超高效液相色谱-同位素稀释串联质谱法测定蜂蜜中的甲硝唑和氯霉素[J].分析科学学报,2017,33(1):145-148.
[7]刘丽,金鑫,韩凤.反相高效液相色谱法同时测定面痤净软膏中甲硝唑和氯霉素的含量[J].中国医院用药评价与分析,2017,17(8):1083-1084,1088.
[8]赵健全,曹倩,陈霞,等.环境中有机污染物检测技术研究进展[[J/OL].应用化工.https://doi.org/10.16581/j.cnki.issn1671-3206.20181101.003.
[9]Zanjani M R K,Yamini Y,Shariati S,et al.A new liquid-phase microextraction method based on solidification of floating organic drop[J].Anal.Chim.Acta,2007,585(2):286-293.
[10]王莹莹,赵广莹,常青云,等.悬浮固化液相微萃取技术研究进展[J].分析化学,2010,38(10):1517-1522.
[11]常青云,周欣,高书涛等.悬浮固化液相微萃取-气相色谱联用测定水样中酰胺类除草剂残留[J].分析化学,2012,40(4):523-528.
[12]卢巧梅,张文敏,黄川辉,等.悬浮固化液相微萃取-高效液相色谱法分析生长素[J].福州大学学报(自然科学版),2015,43(4):554-559.