目的 建立测定牛肺表面活性提取物中多种四环素类抗生素残留的方法。方法 采用UPLC-MS/MS方法,以Waters HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)为固定相,分别以含0.1%甲酸的乙腈溶液和0.1%甲酸的水溶液为流动相A和流动相B,梯度洗脱,流速0.3 mL·min-1,柱温30 ℃,进样量1 μL。结果 该方法能同时测定四环素、金霉素、土霉素、多西环素、美他环素、米诺环素、β-多西环素、差向四环素、差向金霉素、脱水四环素和脱水差向四环素等11种抗生素。各化合物线性范围、灵敏度、精密度、回收率均满足分析要求。在牛肺表面活性提取物中可检出土霉素和四环素,其中土霉素残留量约为0.03 mg·kg-1,四环素则未达到定量限(0.006 mg·kg-1)。结论 该方法可作为检测牛肺表面活性提取物中四环素类抗生素残留的方法。
Abstract
OBJECTIVE To establish a method for the determination of various tetracycline antibiotics residues in calf pulmonary surfactant extract. METHODS UPLC-MS/MS method was adopted with, Waters HSS T3 column(2.1 mm×100 mm,1.8 μm) as solid phase. A acetonitrile solution(containing 0.1% formic acid) and aqueous solution(containing 0.1% formic acid) were used as mobile phase A and mobile phase B, respectively. Gradient elution was conducted at, the flow rate of 0.3 mL·min-1, the column temperature was maintained at 30 ℃, and the injection volume was 1 μL. RESULTS This method can simultaneously determine 11 antibiotics, including tetracycline, chlortetracycline, oxytetracycline, doxycycline, metacycline, minocycline, β-doxycycline, epi-tetracycline, epi-chlortetracycline, anhydrotetracycline, and epi-anhydrotetracycline. The linear range, sensitivity, precision and recoveries of each compound meet the analytical requirements. Tetracycline and oxytetracycline were detected in the calf pulmonary surfactant extract samples. The amount of oxytetracycline residues was about 0.03 mg·kg-1, and the tetracycline did not reach the limit of quantitation(0.006 mg·kg-1). CONCLUSION The method can be used for detecting tetracycline antibiotic residues in calf pulmonary surfactant extract.
关键词
四环素类 /
抗生素 /
残留 /
超高效液相色谱串联质谱法 /
牛肺表面活性提取物 /
固相萃取
{{custom_keyword}} /
Key words
tetracycline /
antibiotics /
residue /
UPLC-MS/MS /
calf pulmonary surfactant extract /
solid phase extraction
{{custom_keyword}} /
中图分类号：
R917
{{custom_clc.code}}
({{custom_clc.text}})
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] LIU X C, DONG Y H, WANG H. Investigation on the residues of tetracycline antibiotics in intensive excavity of livestock and poultry in Jiangsu province[J]. J Argo-Environ Sci(农业环境科学学报), 2008,27(3):1177-1182.
[2] WU L Q, QIAN M R, LU L Z, et al. Antibiotic residues in waste waters from main livestock farms in Zhejiang province[J]. Acta Agric Zhejiangensis(浙江农业学报), 2012,24(4):699-705.
[3] ZHANG L H, WANG J J, HA X J, et al. Distribution characteristics of antibiotic resistance genes in vegetable soils in Beijing[J]. Chin J Environ Sci(环境科学), 2016, 37(11):4395-4401.
[4] Ch.P(2015) Vol IV(中国药典2015年版. 四部)[S]. 2015: 252.
[5] SPIELMEYER A, AHLBORN J, HAMSCHER G. Simultaneous determination of 14 sulfonamides and tetracyclines in biogas plants by liquid-liquid-extraction and liquid chromatograph tandem mass spectrometry[J]. Anal Bioanal Chem,2014,406(11):2513-2524.
[6] DONE H Y, HALDEN R U. Reconnaissance of 47 antibiotics and associated microbial risks in seafood sold in the United States[J]. J Haz Mat,2015,282(SI):10-17.
[7] MOOKANTSA S O S, DUBE S, NINDI M M. Development and application of a dispersive liquid-liquid microextraction method for the determination of tetracyclines in beef by liquid chromatography mass spectrometry[J]. Talanta, 2016, 148:321-328.
[8] BOURDAT-DESCHAMPS M, LEANG S, BERNET N, et al. Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry: optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction[J]. J Chromatogr A, 2014, 1349:11-23.
[9] SHU L. Study on composition analysis and quality control of medicinal calf pulmonary surfactant[D]. Beijing: University of Chinese Academy of Sciences, 2016.
[10] SWEET D G, CARNIELLI V, GREISEN G, et al. Guidelines for the prevention and treatment of neonatal respiratory distress syndrome in Europe[J]. Chin J Pediatr(中华儿科杂志), 2011, 49(1):27-33.
[11] DONG S H. Application of pulmonary surfactant in neonatal respiratory distress syndrome[J]. Chin J Pract Pediatr(中国实用儿科杂志), 1988,3(1):11-12.
[12] LI J, FAN X M, SONG G W, et al. A multicenter clinical trial of the surfactant replacement therapy for neonatal respiratory distress syndrome[J]. Chin J Pediatr(中华儿科杂志), 2000, 38(6):344-347.
[13] ZHANG M, ZHOU X. Neonatal respiratory distress syndrome treatment drug-curosurf[J]. World Pharmacy(国外医药-合成药·生化药·制剂分册), 2001,22(2):110.
[14] XIN Y, ZHENG R X. Clinical analysis of 27 cases of neonatal respiratory distress syndrome complicated with pneumothorax[J]. J Capit Univ Med Sci(首都医科大学学报), 2016,37(2):148-152.
[15] CORBET A J, LONG W A, MURPHY D J, et al. Reduced mortality in small premature infants treated at birth with a single dose of synthetic surfactant[J]. J Paediatr Child Health, 1991, 27:245-249.
[16] ZHANG W T, FU D C, WANG Y. Clinical treatment and analysis of 308 cases of neonatal respiratory distress syndrome[J]. Chin J Pharm Econom(中国药物经济学), 2013,4:321-322.
[17] AVERY M E, MEAD J. Surface properties in relation to atelectasis and hyaline membrane disease[J]. AMA J Dis Child, 1959, 97(5):517-523.
[18] YU J L. Prevention and treatment of neonatal respiratory distress syndrome[J]. Chin J Pract Pediatr(中国实用儿科杂志), 2003, 18(11):643-646.
[19] XU Z Z. Neonatal respiratory distress syndrome[J]. Jiangsu Med J(江苏医药), 1982,5:26-28.
[20] CHEN A, SHI L P, ZHENG J Y, et al. Clinical characteristics and outcomes of respiratory distress syndrome in term and late-preterm neonates[J]. Chin J Pediatr(中华儿科杂志), 2008,46(9):654-657.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}
PDF(2232 KB)
