汤料中罂粟壳成分检测前处理研究  

Research on Pre-Treatment for Detection of Poppy Shell Components in Soup

作　　者：许琨琨 蔡振世 林晓明 王晓峰 吴芳海 XU Kunkun;CAI Zhenshi;LIN Xiaoming;WANG Xiaofeng;WU Fanghai(Quanzhou Institute for Food and Drug Control,Quanzhou 362000,China)

机构地区：[1]泉州市食品药品检验所,福建泉州362000

出　　处：《食品科技》2024年第11期334-342,共9页Food Science and Technology

基　　金：泉州市2021年科技计划项目(2021N184S)。

摘　　要：目的:比较不同的净化滤材用于表面增强拉曼技术(Surface-enhanced Raman spectroscopy,SERS)和超高效液相色谱-串联质谱法(Ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS-MS)测定餐饮汤料中罂粟壳成分时的差异。方法:UPLC-MS-MS采用ACQUITY UPLC■BEH HILIC C_(18)色谱柱,使用0.1%甲酸的10 mmol/L乙酸铵溶液与0.1%甲酸的乙腈溶液进行梯度洗脱,流速为0.3 mL/min;SERS采用激光波长为785 nm,激光功率为250 mW。结果:采用UPLC-MS-MS方法检测罂粟壳中5种成分,自混合滤材平均回收率为65.4%~97.1%,CQ11-3滤材平均回收率为69.3%~87.9%,6550HP平均回收率为43.4%~109.8%,3150-VD滤材平均回收率为72.7%~103.8%,3150-VDS滤材平均回收率为85.7%~104.7%,QVet-NM+平均回收率为12.4%~104.3%,QVet-HP+滤材平均回收率为23.2%~102.1%,AOAC平均回收率为69.6%~86.5%,Captiva EMR-Lipid滤材平均回收率为74.0%~92.5%,EMR-GPD with Carbon S滤材平均回收率为64.2%~80.8%,Styra MCX滤材平均回收率为73.6%~98.2%。采用SERS方法QuEChERS滤材CQ11-3和AOAC、推杆式QuEChERS滤材3150-VDS和3150-VD、固相萃取柱滤材Styra MCX和Captiva EMR-Lipid检出限为40~80μg/kg,其余滤材的检出限为160μg/kg。自混合滤材和QuEChERS滤材的平均检验用时约9.75 min,推杆式QuEChERS滤材的平均检验用时6~7 min,固相萃取柱滤材的平均检验用时约为18 min。结论:推杆式QuEChERS配合SERS方法可实现汤料中罂粟壳5种生物碱类物质的快速检测,检出限和准确度均能满足检测需要。如果检出结果为阳性,则可用UPLC-MS-MS方法进行验证。Objective:To compare the differences in the use of different purification filter materials for surface enhanced Raman spectroscopy(SERS)and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS)determination of poppy shell components in food soup.Methods:UPLCMS-MS adopted ACQUITY UPLC®BEH HILIC C_(18) chromatography column,gradient elution of 10 mmol/L ammonium acetate solution with 0.1%formic acid and 0.1%formic acid acetonitrile solution at a flow rate of 0.3 mL/min.A laser wavelength of 785 nm and a laser power of 250 mW were used in SERS method.Result:In the UPLC-MS/MS method,the average recovery rates for 5 components in poppy shell were as follows:65.4%to 97.1%for self-mixed filter media,69.3%to 87.9%for CQ11-3 filter media,43.4%to 109.8%for 6550HP filter media,72.7%to 103.8%for 3150-VD filter media,85.7%to 102.6%for 3150-VDS filter media,12.4%to 104.3%for QVet-NM+filter media,23.2%to 102.1%for QVet-HP+filter media,69.6%to 86.5%for AOAC filter media,74.0%to 92.5%for Captiva EMR-Lipid filter media,64.2%to 80.8%for EMR-GPD with Carbon S filter media,and 73.6%to 98.2%for Styra MCX filter media.In the SERS method,the detection limits for QuEChERS filter materials CQ11-3 and AOAC,push-type QuEChERS filter materials 3150-VDS and 3150-VD,and solid phase extraction(SPE)column filter materials Styra MCX and Captiva EMR-Lipid were 40–80μg/kg,while the detection limits for other filter materials were 160μg/kg.The average test time for self-mixed and QuEChERS filter materials was approximately 9.75 minutes,the average test time for push-type QuEChERS filter materials was approximately 6–7 minutes,and the average test time for SPE column filter materials was approximately 18 minutes.Conclusion:The push-type QuEChERS combined with the SERS method enables the rapid detection of five alkaloid compounds in poppy shells in soup stock.The detection limits and accuracy meet the required detection standards.If the result is positive,the UPLC-MS-MS method can be used for confirmation.

关 键 词：表面增强拉曼技术 QUECHERS 超高效液相色谱-串联质谱法 罂粟壳 快速检验 

分 类 号：TS207.5[轻工技术与工程—食品科学]