超高效液相色谱-质谱法测定猪肉中9种β—受体激动剂残留量 .pdfVIP

超高效液相色谱-质谱法测定猪肉中9种β—受体激动剂残留

量

曾绍东;王明月;杨春亮;查玉兵;林玲

【摘要】优化提取猪肉中9种β-受体激动剂的酶解条件,并建立同时测定猪肉中9

种β-受体激动剂的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法.样品经β-

盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解、异丙醇-乙酸乙醇溶液(6∶4)提取、MCX

固相萃取柱净化,以乙腈-0.1％甲酸水溶液为流动相,C18柱为色谱柱进行分离,串联

质谱正离子多反应监测(MRM)模式测定,内标法定量.结果表明,β-盐酸葡萄糖醛苷

酶/芳基硫酸酯酶的最佳酶解条件为每克猪肉中酶添加量为2500U,酶解时间为

6.0h.9种β-受体激动剂在0.25～10μg/L范围内有良好的线性关系,检出限为

0.2μg/kg,定量限为0.5μg/kg;在3种添加水平下,样品平均回收率在80.4％～

110.3％之间,相对标准偏差≤6.7％.该方法缩短了样品前处理时间,具有良好的灵敏

度和准确性,尤其适合大批量猪肉样品中9种β-受体激动剂的快速确证和定量分

析.%Theenzymatichydrolysisparametersforextractnineβ-agonistsin

porkwasoptimizedandamethodforsimultaneousdeterminationofnine

β-agonistsresiduesinporkbyultra-performanceliquidchromatography-

massspectrometry(UPLC-MS/MS)wasestablished.Thesampleswere

enzymehydrolysisedbyβ-Glucuronidase/arylsulfatase,extractedwith

isopropanol-ethylacetate(6..4),andcleanuponaMCXSPE

cartridge,separatedonaC18columnusingacetonitrile-0.1％formicacid

solutionasmobilephase,andthendetectedundermultiplereaction

monitoring(MRM)mode.Theresultsshowedthattheoptimumconditions

wasobtainedbyhydrolysisfor6.0husingβ-Glucuronidase/arylsulfataseat

37℃,pH=5.2,enzymedosage2500U/g·sample.Themethodshoweda

goodlinearityforalltheanalytesovertherangeof0.25-10μg/L.The

detectionlimitsandquantitationlimitswere2.0μg/kgand5.0μg/kg

respectively.Therecoveriesrangedfrom80.4％to110.3％atthreespiked

concentrationswiththerelativestandarddeviations≤6.7％.Theresults

establishedthatsuchamethodhastheadvantagesoftime-saving,fastto

perform,withhighsensitivityandaccuracy,anditissuitablefordetectionof

nineβ-agonistsresiduesinpork,especiallyforarapidconfirmatoryand

quantitativeanalysis.

【期刊名称】《分析仪器》

【年(卷),期】2013(000)004

【总页数】7页(P5-11)

【关键词】超高效液相色谱-串联质谱;猪肉;β-受体激动剂

【作者】曾绍东;王明月;杨春亮;查玉兵;林玲

【作者单位】中国热带农业科学院农产品加工研究所,湛江524001;中国热带农业

科