液相色谱-紫外检测法和液相色谱-质谱联用法同时测定小麦中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇的实验室间研究

Interlaboratory study of LC-UV and LC-MS methods for the simultaneous determination of deoxynivalenol and nivalenol in wheat.

作者信息

Aoyama Koji, Akashi Hajime, Mochizuki Naoki, Ito Yuji, Miyashita Takashi, Lee Soohyung, Ogiso Motoki, Maeda Mamoru, Kai Shigemi, Tanaka Hiroki, Noriduki Hiroko, Hiraoka Hisaaki, Tanaka Toshitsugu, Ishikuro Eiichi, Itoh Yoshinori, Nagayama Toshihiro, Nakajima Masahiro, Naito Shigehiro, Sugita-Konishi Yoshiko

机构信息

Food and Agricultural Materials Inspection Center, Sendai, Japan.

出版信息

Shokuhin Eiseigaku Zasshi. 2012;53(3):152-6. doi: 10.3358/shokueishi.53.152.

DOI:10.3358/shokueishi.53.152

PMID:22790717

Abstract

To evaluate LC methods with UV or MS detection for simultaneous analysis of deoxynivalenol (DON) and nivalenol (NIV) in wheat, an interlaboratory study was conducted in 11 laboratories. DON and NIV were purified using a multifunctional column, and their concentrations were determined using LC-UV or LC-MS(/MS). No internal standards were used. Three fortified wheat samples (0.1, 0.5 and 1 mg/kg), one naturally contaminated wheat sample, and one blank wheat sample were used. The recoveries ranged from 90% to 110% for DON and from 76% to 83% for NIV. For DON, the relative standard deviations for repeatability (RSDr) ranged from 1.1% to 7.6%. The relative standard deviations for reproducibility (RSDr) ranged from 7.2% to 25.2%. For NIV, the RSDr ranged from 2.0% to 10.7%, and the RSDr ranged from 7.0% to 31.4%. Regardless of sample and detector, the HorRat values for DON and NIV ranged from 0.4 to 1.4. Both LC-UV and LC-MS(/MS) methods were considered to be suitable for application as an official method.

摘要

为评估采用紫外或质谱检测的液相色谱法同时分析小麦中的脱氧雪腐镰刀菌烯醇（DON）和雪腐镰刀菌烯醇（NIV），在11个实验室开展了一项实验室间研究。DON和NIV使用多功能柱进行净化，其浓度采用液相色谱 - 紫外或液相色谱 - 质谱（/质谱）测定。未使用内标。使用了三个加标小麦样品（0.1、0.5和1 mg/kg）、一个天然污染小麦样品和一个空白小麦样品。DON的回收率在90%至110%之间，NIV的回收率在76%至83%之间。对于DON，重复性相对标准偏差（RSDr）在1.1%至7.6%之间。再现性相对标准偏差（RSDr）在7.2%至25.2%之间。对于NIV，RSDr在2.0%至10.7%之间，RSDr在7.0%至31.4%之间。无论样品和检测器如何，DON和NIV的HorRat值在0.4至1.4之间。液相色谱 - 紫外和液相色谱 - 质谱（/质谱）方法均被认为适用于作为官方方法应用。