超高效液相色谱-四极杆飞行时间质谱法快速测定畜禽产品中抗组胺类药物残留

王京; 叶佳明; 钟世欢; 王潇; 陈青俊

doi:10.13386/j.issn1002-0306.2020050044

超高效液相色谱-四极杆飞行时间质谱法快速测定畜禽产品中抗组胺类药物残留

王京^1,2,
叶佳明¹,
钟世欢¹,
王潇¹,
陈青俊^3, ,

1. 赞宇科技集团股份有限公司, 浙江杭州 310030;
2. 浙江省轻工业研究所, 浙江杭州 310009;
3. 浙江公正检验中心有限公司, 浙江杭州 311305

基金项目:

浙江省公益技术研究计划项目（LGN18B050001）。

详细信息

作者简介:
王京(1987-),男,硕士研究生,高级工程师,研究方向:食品安全,E-mail:178058645@qq.com。

通讯作者:
陈青俊(1970-),男,本科,高级工程师,研究方向:食品安全,E-mail:1656484445@qq.com。

中图分类号: TS207.3
计量
- 文章访问数: 205
- HTML全文浏览量: 19
- PDF下载量: 17
出版历程
- 收稿日期: 2020-05-05
- 网络出版日期: 2021-03-02
- 刊出日期: 2021-02-28

Determination of Antihistamine Residues in Livestock and Poultry Products by Ultra Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

1. Zanyu Technology Group Co., Ltd., Hangzhou 310030, China;
2. Zhejiang Institute of Light Industry, Hangzhou 310009, China;
3. Zhejiang Gongzheng Inspection Center Co., Ltd., Hangzhou 311305, China

摘要

摘要: 建立超高效液相色谱-四极杆飞行时间质谱（UPLC-Q-TOF/MS）快速测定畜禽产品中19种抗组胺类药物及代谢物残留的方法。样品用乙腈-乙酸乙酯溶液提取，提取液经增强型脂质去除剂（EMR）结合经氧化修饰的多壁碳纳米管（MWCNTs）净化，以0.1%甲酸水-0.1%甲酸乙腈作为流动相进行梯度洗脱，在EclipsePlus-C₁₈（50 mm×2.1 mm，1.8 μm）色谱柱上分离，柱温40℃，流速0.3 mL/min，进样量5 μL，Q-TOF/MS电喷雾正离子模式分析检测。在全扫描模式下采集一级质谱数据，以待测物的准分子离子峰的峰面积定量，以保留时间、精确质量数、同位素丰度比等特征信息定性。在Target MS/MS模式下靶向采集二级质谱数据，通过特征碎片离子的精确质量数等信息进一步确证。结果表明，所有药物在浓度范围内线性良好，决定系数均大于0.996，不同阴性样品基质中（牛肉、鸡肉、猪肝）在3个浓度水平加标试验回收率在78.2%~105.3%之间，相对标准偏差（RSD）为3.2%~8.2%，方法检出限（LOD，S/N≥3）为0.5~2.0 μg/kg，定量限为1.5~6.0 μg/kg。本方法简便快速，灵敏度高，选择性好，结果准确，适用于畜禽产品中19种抗组胺类药物及代谢物的快速筛查和定量测定。
- 抗组胺药物 /
- 超高效液相色谱-四极杆飞行时间质谱 /
- 增强型脂质去除吸附剂 /
- 多壁碳纳米管
Abstract: A rapid method for the determination of 19 antihistamines and metabolites residues in livestock and poultry products by UPLC-Q-TOF/MS was developed. Samples,were extracted with acetonitrile-ethyl acetate solution extract by enhanced matrix removal(EMR)combined with oxidative modification of multi-walled carbon nanotubes(MWCNTs)purification,with 0.1% formic acid formic acid water-0.1% acetonitrile as mobile phase in gradient elution,in EclipsePlus-C₁₈(50 mm×2.1 mm,1.8 μm)on the chromatographic column separation,column temperature 40 ℃,the flow rate of 0.3 mL/min,sample quantity was 5 μL,Q-TOF/MS electrospray cations pattern analysis. The first-order mass spectrometry data were collected in the full-scan mode to quantify the peak area of the excimer ion peak of the measured object,and to determine the quality of the characteristic information such as retention time,accurate mass number and isotope abundance ratio. In the Target MS/MS mode,the secondary mass spectrometry data were targeted and further confirmed by the accurate mass number of the characteristic fragment ions. Statistics indicated that this method whose RSD was 3.2%~8.2%,had a good linear with R²>0.996 in their ranges of linearity,what’s more,the LODs of which were 0.5~2.0 μg/kg and the LOQs were 1.5~6.0 μg/kg along with a hige recovery rate ranged 78.2%~105.3% from different sample matrixes(beef,chicken,pork liver)added 3 levels of concentration.. This method is simple,rapid,sensitive,selective and accurate,and is suitable for rapid screening and quantitative determination of 19 antihistamines and metabolites in livestock and poultry products.

HTML全文

参考文献(21)

[1]	闫小峰. 浅谈我国兽药行业存在的主要问题及对策[J]. 中国兽药杂志,2009,43(8):35-38.
[2]	潘明飞,王俊平,方国臻,等. 食品中农兽药残留检测新技术研究进展[J]. 食品科学,2014,35(15):277-282.
[3]	Yadollah Yamini,Mohammad Faraji. Extraction and determination of trace amounts of chlorpromazine in biological fluids using magnetic solid phase extraction followed by HPLC[J].Journal of Pharmaceutical Analysis,2014,4(4):279-285.
[4]	叶林虎,徐松,王丽莎,等. LC-MS/MS法检测皮肤科常用中药制剂中添加的7种抗组胺药物[J]. 药物分析杂志,2016,36(11):2022.
[5]	齐士林,吴敏,严丽娟,等. 超高效液相色谱-质谱对动物源食品中氯丙嗪、异丙嗪及其代谢物的测定[J]. 分析测式学报,2009,28(6):677-681.
[6]	王伟,陈振玲,崔玉静,等. 超高效液相色谱质谱法同时测定人血浆中8种抗组胺类药物[J]. 中国临床药理学杂志,2017,33(10):929-932.
[7]	Li M,Kong W,Li Y,et al. High-throughput determination of multi-mycotoxins in Chinese yamand related products by ultra fast liquid chromatography coupled with tandem mass spectrometry after one-step extraction[J]. J Chromatogr B,2016,1022(6):118-125.
[8]	Lozowicka B,Rutkowska E,Jankowska M. Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD[J]. Environmental Science and Pollution Research,2017,24(8):7124-7138.
[9]	李琴,陶大利,周红,等. 超高效液相-串联质谱法同时测定生鲜乳中45种兽药残留量[J]. 中国乳品工业,2016,44(1):44-47.
[10]	梁玉禧,李益珍,等. 液质联用法测定猪肉产品中违禁添加物氯丙嗪、异丙嗪和万古霉素残留研究[J]. 粮食与饲料工业,2016(2):69-73.
[11]	李志刚,任南,马燕红,等. 高效液相色谱-串联质谱法检测鲜冻肉中违禁注水药物[J]. 食品科学,2018,39(12):308-312.
[12]	谢寒冰,蒋万枫,赵海峰,等. 高效液相色谱法-四极杆飞行时间质谱法测定猪肉中20种兽药残留量[J]. 理化检验(化学分册),2014,50(6 ):702-707.
[13]	程建桥,王传胜,张峰,等. 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定猪肉中氯丙嗪及其代谢物[J].食品安全质量测试学报,2018,9(10):2440-2445.
[14]	颜春荣,张波,方萍,等. 猪肉中19种β-受体激动剂的液相色谱串联四极杆-飞行时间质谱(Q-TOF)筛查和确证方法研究[J]. 分析试验室,2015,34(1):35-39.
[15]	杨盛茹,李颖,蔡英华,等. 使用超高效液相色谱-串联飞行时间质谱(Q-Tof)和UNIFI筛查软件进行动物尿液中兽药及违禁药物筛查分析[J]. 分析试验室,2017,36(4):418-422.
[16]	Jessica J W Broeders,Bas J Blaauboer,Joop M Hermens. Development of a negligible depletion-solid phase microextraetion method to determine the free concentration of chlorpromazine inaqueous samples containing albumin[J]. Chromatography A,2011,1218:8529-8535.
[17]	Wejdan S K,Bahruddin S,Normaliza H A,et al. Micro-solid phase extraction with liquid chromatograph-tandem mass spectrometry for the determination of aflatoxins in coffee and malt beverage[J]. Food Chem,2014,147(4):287-294.
[18]	孙伟华,杨欢,曹赵云,等. 基于分散固相萃取液相色谱-串联质谱法测定大米中8种真菌毒素[J]. 分析测试学报,2017,36(1):47-53.
[19]	陈晓鹏,顾采琴,张施敬,等. QuEChERS-UPLC-MS/MS同时测定牛奶和奶粉中42种类固醇激素[J]. 食品科学,2018,39(8):314-321.
[20]	Calatayud-Vernich P,Calatayud F,Simo E,et al. Efficiency of QuEChERS approach for determining 52 pesticide residues in honey and honey bees[J]. Methods X,2016(3):452-458.
[21]	王京,叶佳明,王潇,等. 空间位阻净化-超高效液相色谱-串联质谱技术测定动物源性食品中抗组胺类药物残留[J]. 食品科学,2019,40(12):345-352.