A method for the simultaneous determination of 18 sulfonamides in antler velvet of Cervus by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed by using the pretreatment technology of dispersed solid-phase extraction. Antler samples were extracted with acetonitrile and purified with 70 mg PSA, 100 mg C18 and 50 mg neutral alumina. The UPLC analysis was carried out by a 35 ℃ thermostatic Waters Acquity UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm)with a mobile phase composed of 25 mmol/L formic acid acetonitrile-water for gradient elution at 0.3 mL/min. The detection was carried out on MS/MS with ESI in positive ion in the multiple reaction monitoring (MRM) mode. The content of sulfonamides in anter velvet was quantified by external standard method. The results showed that 18 varieties of sulfonamides had a good linear relationship between 0.025-50 ng/mL; the correlation coefficient R2 were all greater than 0.999 1; limit of detection (LOD) of 7 kinds of sulfonamides was 0.025 μg/kg; limit of quantitation (LOQ) was 0.075 μg/kg; LOD of 11 kinds of sulfonamides was 0.075 μg/kg; and LOQ was 0.25 μg/kg. The average recovery of 18 sulfonamides was 80.4%-107.2% with relative standard deviation (RSD) less than 5%. The method has the advantages of simple operation, remarkable purification effect, high sensitivity, good accuracy and low detection limit. It can be used for the determination of 18 sulfonamides in antler velvet of Cervus Nippon Temminck.
HUANG Shengguang
,
ZHAO Hui
,
WANG Yufang
,
JIN Meiling
,
SONG Chao
,
WANG Feng
. Determination of 18 kinds of sulfonamides in antler velvet of Cervus nippon Temminck by QuEChERS/UPLC-MS/MS[J]. Food and Fermentation Industries, 2019
, 45(24)
: 223
-228
.
DOI: 10.13995/j.cnki.11-1802/ts.021835
[1] 国家药典委员会. 中华人民共和国药典: 2015年版. 一部[S]. 北京:中国医药科技出版社,2015: 323-324.
[2] 孙亚奇,郭京超,潘源虎,等. 磺胺类药物代谢与残留消除以及检测方法研究进展[J]. 中国兽药杂志,2019,53(2):66-75.
[3] 于淼. 养殖业中磺胺类药物残留的危害及现状[J]. 现代畜牧科技,2015,29(2):133.
[4] 中华人民共和国农业农村部.动物性食品中兽药最高残留限量(农业农村部2002年235号公告)[EB/OL].[2012-12-24]. http://moa.gov.cn/gk/tzgg-1/gg/200302/t20030226.59300.htm.
[5] 赵晓凤,杨中. 气相色谱-串联质谱法检测猪肉组织中的磺胺二甲嘧啶残留量[J]. 饲料工业,2007,28(2):54-57.
[6] 廖春蓉,郭雅蓉. 气相色谱-串联质谱法检测葡萄中苯氟磺胺和甲苯氟磺胺残留量[J]. 医学动物防制,2017,33(2):236-238.
[7] 李仪,张炎,张雅婷,等. 微萃取超高效液相色谱检测磺胺类药物的研究[J]. 华东师范大学学报(自然科学版),2019,204(2):156-163.
[8] 杨舒婷,林伟锐,梁建华,等. 固相萃取-高效液相色谱法测定水中磺胺二甲基嘧啶、磺胺甲基异噁唑的方法探究[J]. 肇庆学院学报,2019,40(2):46-50.
[9] 段羚. 高效液相色谱法测定饮料中乙酰磺胺酸钾含量的不确定度分析[J]. 现代食品,2018,31(20):91-95.
[10] 冯涛,刘道中,章安源,等. 高效液相色谱法测定恩诺沙星注射液中的磺胺类药物[J]. 山东畜牧兽医,2019,40(1):3-5.
[11] 周靖雯,吴友谊,殷斌. 中空纤维膜液相微萃取-毛细管电泳法测定环境水样中的4种磺胺类药物[J]. 理化检验-化学分册,2018,54(6):627-633.
[12] 陈建,杨灵芝,张金金,等. 毛细管电泳法分离9种磺胺类药物[J]. 分析仪器,2018,42(3):51-56.
[13] 韩燕祯,朱怀娇,石红梅,等. 高效毛细管电泳法测定泳池中尿液指示物乙酰磺胺酸钾[J]. 分析测试学报,2018,37(7):854-857.
[14] 黄学泓,陈燕勤,林文. 酶联免疫分析法测定猪肠衣中磺胺二甲基嘧啶残留量[J]. 检验检疫学刊,2011,21(4):21-22;52.
[15] 刘超,韩世泉,刘一兵. 广谱检测磺胺类药物的酶联免疫分析方法的建立[J]. 标记免疫分析与临床,2012,19(5):286-290.
[16] 蒋文晓. 动物性食品中喹噁啉类药物代谢物和磺胺类—喹诺酮类药物多残留免疫分析方法研究[D]. 北京:中国农业大学,2014.
[17] 王欣梅,徐桂菊,王晓利,等. 三聚氰胺/邻苯二甲醛共价有机骨架材料结合固相萃取-液相色谱串联质谱检测环境水样中痕量磺胺类抗生素[J]. 分析化学,2018,46(12):149-155.
[18] 刘小燕,高仕谦,丁阳杰,等. 离子液体磁性石墨烯-超高效液相色谱串联质谱法测定水中的磺胺类抗生素[J]. 现代化工, 2019,54(5):246-250;252.
[19] 刘桂英,宋广军,王召会,等. 固相萃取-超高效液相色谱串联质谱法测定水产品中磺胺类药物残留[J]. 食品安全质量检测学报,2019,25(8):2 240-2 246.
[20] 钱卓真,汤水粉,梁焱,等. QuEChERS-高效液相色谱-串联质谱法同时测定水产养殖环境沉积物中磺胺类、喹诺酮类、大环内酯类抗生素[J]. 质谱学报,2019,30(4):356-368.
[21] KIM L, LEE D, CHO H, et al. Review of the QuEChERS method for the analysis of organic pollutants: Persistent organic pollutants, polycyclic aromatic hydrocarbons, and pharmaceuticals[J]. Trends in Environmental Analytical Chemistry, 2019, 25(12):2 247-2 256.
[22] PERESTRELO R, SILVA P, PORTO-FIGUEIRA P, et al. QuEChERS - Fundamentals, relevant improvements, applications and future trends[J]. Analytica Chimica Acta,2019, 33(18):2 140-2 146.
[23] DUALIE P, PARDO O, FERNÁNDEZ S F, et al. Determination of four parabens and bisphenols A, F and S in human breast milk using QuEChERS and liquid chromatography coupled to mass spectrometry[J]. Journal of Chromatography B,2019, 1 114:154-166.
