超高效液相-质谱/质谱法测定蜂蜜中的林可霉素残留
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摘要
目的建立蜂蜜中林可霉素残留的高效液相色谱-质谱联用法,并用于江苏五市市售蜂蜜中林可霉素的残留水平检测。方法样品经固相萃取提取净化、反相液相色谱分离后质谱检测,基质匹配标准内标法定量。结果方法在1.0μg/kg～100μg/kg浓度时线性关系良好(r=0.996),检出限为0.2μg/kg,定量限为0.7μg/kg,回收率为92.88%～107.51%,相对标准偏差为4.6%～8.6%。样品中林可霉素的检出率为24%,最大残留量为2.998μg/kg。结论该法简单、灵敏、准确,可用于蜂蜜中林可霉素残留的测定。
Objective To develop an analytical method for the determination of lincomycin in honey by ultra performance liquid chromatography-tandem mass spectrometry and apply the method to the investigation of lincomycin residue in honey from five cities of Jiangsu Province. Methods The sample was extracted and purified with solid-phase extraction and then separated with reversed-phase ultra performance liquid chromatography and detected by electro spray tandem mass spectrometry in the MRM mode. Quantification was based on internal standard with matrix-matched calibration standard curve. Results The linearity for lincomycin ranged from 1.0 μg/kg-100 μg/kg with the correlation coefficient(r) greater than 0.996. The limit of detection(LOD) of lincomycin was 0.2 μg/kg, and the limit of quantification(LOQ) was 0.7 μg/kg. The recoveries were within 92.88%-107.51% with the relative standard deviations of 4.6%-8.6%. The positive rate of lincomycin in 50 samples was 24%, and the highest content was 2.998 μg/kg. Conclusion The method is simple, sensitive, accurate, and it can be applied to the determination of lincomycin in honey.
Objective To develop an analytical method for the determination of lincomycin in honey by ultra performance liquid chromatography-tandem mass spectrometry and apply the method to the investigation of lincomycin residue in honey from five cities of Jiangsu Province. Methods The sample was extracted and purified with solid-phase extraction and then separated with reversed-phase ultra performance liquid chromatography and detected by electro spray tandem mass spectrometry in the MRM mode. Quantification was based on internal standard with matrix-matched calibration standard curve. Results The linearity for lincomycin ranged from 1.0 μg/kg-100 μg/kg with the correlation coefficient(r) greater than 0.996. The limit of detection(LOD) of lincomycin was 0.2 μg/kg, and the limit of quantification(LOQ) was 0.7 μg/kg. The recoveries were within 92.88%-107.51% with the relative standard deviations of 4.6%-8.6%. The positive rate of lincomycin in 50 samples was 24%, and the highest content was 2.998 μg/kg. Conclusion The method is simple, sensitive, accurate, and it can be applied to the determination of lincomycin in honey.
引文
[1] 周玲.蜂巢及蜂产品中红霉素和林可霉素残留的HPLC-MS/MS分析方法及其变化规律研究[D].北京:中国农业科学院,2013.
[2] 侯建波,谢文,陈笑梅,等.固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留[J].色谱,2011,29(6):535-542.
[3] 陈荣锋.蜂蜜中抗生素残留的归因分析与检测技术概要[J].食品安全导刊,2018(9):108-108.
[4] Thompson TS,Noot DK,Calvert J,et al.Determination of lincomycin and tylosin residues in honey using solid-phase extraction and liquid chromatography-atmospheric pressure chemical ionization mass spectrometry[J].J Chromatogr A,2003,1020(2):241-250.
[5] 阮祥,春曾明,华赵明.HPLC-ESI-MS/MS检测蜂蜜中林可霉素残留[J].安徽农业科学,2009,37(5):1889-1891.
[6] 毛小报,张社梅,柯福艳.浙江省蜂产业研究状况、成就、问题及对策[J].中国蜂业,2010,61(3):45-46.
[7] Tolgyesi A,Fekete J,Fekete S,et al.Analysis of sub mug/kg lincomycin in honey,muscle,milk,and eggs using fast liquid chromatography-tandem mass spectrometry[J].J Chromatogr Sci,2012,50(3):190-198.
[8] Bogdanov S.Contaminants of bee products[J].Apidologie,2006,37(1):1-18.
[9] Dousa M,Sikac Z,Halama M,et al.HPLC determination of lincomycin in premixes and feedstuffs with solid-phase extraction on HLB OASIS and LC-MS/MS[J].J Pharmaceut Biomed,2006,40(4):981-986.
[10] 冯强.浙江省蜂蜜中主要抗生素及重金属残留的风险评估及检测方法的研究[D].杭州:浙江工业大学,2013.
[11] 徐锦忠,吴斌,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蜂蜜中的林可胺类抗生素残留[J].色谱,2006,24(5):436-439.
[12] 郑荣,王柯.除螨祛痘类化妆品中林可霉素和克林霉素的测定[J].中国卫生检验杂志,2014,24(5):677-678,681.
[13] 林洁,曹建明,蔡欣欣,等.超高效液相色谱三重四极杆质谱法快速测定蜂蜜中12种大环内酯和林可酰胺类药物残留[J].中国卫生检验杂志,2010,20(5):959-962.
[14] 张燕惠,李玲玲,王红梅.高效液相色谱-串联质谱法测定化妆品中10种抗生素[J].中国卫生检验杂志,2017,27(18):2600-2602.
[15] Benetti C,Piro R,Binato G,et al.Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS)[J].Food Addit Contama,2006,23(11):1099-1108.
[2] 侯建波,谢文,陈笑梅,等.固相萃取-液相色谱-质谱/质谱法同时测定蜂蜜中的多类药物残留[J].色谱,2011,29(6):535-542.
[3] 陈荣锋.蜂蜜中抗生素残留的归因分析与检测技术概要[J].食品安全导刊,2018(9):108-108.
[4] Thompson TS,Noot DK,Calvert J,et al.Determination of lincomycin and tylosin residues in honey using solid-phase extraction and liquid chromatography-atmospheric pressure chemical ionization mass spectrometry[J].J Chromatogr A,2003,1020(2):241-250.
[5] 阮祥,春曾明,华赵明.HPLC-ESI-MS/MS检测蜂蜜中林可霉素残留[J].安徽农业科学,2009,37(5):1889-1891.
[6] 毛小报,张社梅,柯福艳.浙江省蜂产业研究状况、成就、问题及对策[J].中国蜂业,2010,61(3):45-46.
[7] Tolgyesi A,Fekete J,Fekete S,et al.Analysis of sub mug/kg lincomycin in honey,muscle,milk,and eggs using fast liquid chromatography-tandem mass spectrometry[J].J Chromatogr Sci,2012,50(3):190-198.
[8] Bogdanov S.Contaminants of bee products[J].Apidologie,2006,37(1):1-18.
[9] Dousa M,Sikac Z,Halama M,et al.HPLC determination of lincomycin in premixes and feedstuffs with solid-phase extraction on HLB OASIS and LC-MS/MS[J].J Pharmaceut Biomed,2006,40(4):981-986.
[10] 冯强.浙江省蜂蜜中主要抗生素及重金属残留的风险评估及检测方法的研究[D].杭州:浙江工业大学,2013.
[11] 徐锦忠,吴斌,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蜂蜜中的林可胺类抗生素残留[J].色谱,2006,24(5):436-439.
[12] 郑荣,王柯.除螨祛痘类化妆品中林可霉素和克林霉素的测定[J].中国卫生检验杂志,2014,24(5):677-678,681.
[13] 林洁,曹建明,蔡欣欣,等.超高效液相色谱三重四极杆质谱法快速测定蜂蜜中12种大环内酯和林可酰胺类药物残留[J].中国卫生检验杂志,2010,20(5):959-962.
[14] 张燕惠,李玲玲,王红梅.高效液相色谱-串联质谱法测定化妆品中10种抗生素[J].中国卫生检验杂志,2017,27(18):2600-2602.
[15] Benetti C,Piro R,Binato G,et al.Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS)[J].Food Addit Contama,2006,23(11):1099-1108.