超高效液相色谱-串联质谱检测猪胆粉中黄曲霉毒素的2种前处理方法比较研究  

Comparison of Two Pretreatment Methods for Determination of Aflatoxin in Suis Fellis Pulvis by UPLC-MS/MS

作　　者：廖予菲[1] 王萍[1] 张瑞瑞[1] 程茜菲[1] LIAO Yufei;WANG Ping;ZHANG Ruirui;CHENG Qianfei(Shaanxi Institute of International Trade&Commerce,Xi’an,Shaanxi 712046 China)

机构地区：[1]陕西国际商贸学院,陕西咸阳712046

出　　处：《陕西农业科学》2022年第8期29-34,共6页Shaanxi Journal of Agricultural Sciences

基　　金：陕西省教育厅科研计划项目(地标药材猪胆膏与国标药材猪胆粉的质量一致性评价编号:21JK0520)。

摘　　要：以中医药传统药物猪胆粉作为研究对象,采用UPLC-MS/MS(超高效液相色谱-串联质谱)作为测定方法,分别通过免疫亲和柱法及QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)法进行样品前处理,通过考察方法的稳定性、重复性、回收率、检测限,对两种前处理方法进行评价。结果表明两种前处理方法所制样品中杂质对四种黄曲霉毒素峰均无干扰,能专属的测定黄曲霉毒素,免疫亲和柱法处理效果更佳,杂质较少。两种方法对黄曲霉毒素G族回收率结果无显著性差异,对黄曲霉毒素B族则QuEChERS法回收率更高。重复性、检测限对比结果,免疫亲和柱法优于QuEChERS法。因此两种前处理方法各有优劣,但整体而言,从操作简便,节约成本的角度来讲,QuEChERS法更优。此研究可为快速高效测定中药中的黄曲霉毒素提供思路,准确快速检验国药,对于“三农”中家畜猪的养殖,充分利用家畜副产品具有重要意义。Comparison of two commonly used pretreatment methods for the determination of aflatoxin. The traditional Chinese medicine Suis Fellis Pulvis p was used as the research object, and UPLC-MS/MS was used as the determination method. The samples were pretreated by immunoaffinity column method and QuEChERS method, respectively. The stability, repeatability, recovery rate and detection limit of the two methods were evaluated. The results showed that the impurities in the samples prepared by the two pretreatment methods had no interference on the four aflatoxin peaks, and could be used to determine aflatoxin exclusively. The immunoaffinity column method had better effect and less impurities. There was no significant difference in the recovery rate of aflatoxin group G between the two methods, but the recovery rate of QuEChERS method was higher for aflatoxin group B. The results of repeatability and detection limit showed that immunoaffinity column method was better than QuEChERS method. The two pretreatment methods had their own advantages and disadvantages, but on the whole, QuEChERS method was better in terms of simple operation and cost saving. This study can provide a reference for the rapid and efficient determination of aflatoxin in traditional Chinese medicine, accurate and rapid detection of traditional Chinese medicine, which is of great significance for the breeding of livestock and pigs and full use of livestock by-products.

关 键 词：黄曲霉毒素 猪胆粉 免疫亲和柱法 样品前处理技术 

分 类 号：R917[医药卫生—药物分析学]