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超高效液相色谱-串联质谱法测定血浆中烷基间苯二酚

作  者:
张雪松;王宇飞;王国栋;向雪松;王竹
单  位:
中国疾病预防控制中心营养与健康所;深圳宝安区中心医院
关键词:
烷基间苯二酚;全麦食品;血浆;超高效液相色谱-串联质谱
摘  要:
目的:建立超高效液相色谱-串联质谱法测定血浆中2种全麦食品生物标志物烷基间苯二酚(ARs)的方法。方法:血浆加入内标,经丙酮提取,离心取上清液过滤,滤液吹干异丙醇定容,使用实心核色谱柱(2. 1mm×100mm,1. 6μm)为分离柱,以异丙醇∶乙腈=30∶70为流动相,等度洗脱,质谱采用电喷雾负离子模式,多反应监测模式进行检测,用内标法定量。结果:2种ARs在2~200ng/mL浓度范围内线性良好,r~2> 0. 998 0。方法检出限为0. 1ng/mL,定量限为0. 3ng/mL,加标回收率为88. 2%~110%,相对标准偏差为2. 48%~13. 2%(n=6)。结论:该方法快速准确、灵敏度高、前处理简单,能够有效测定血浆中2种ARs的含量。
译  名:
Determinnation of Alkylresorcinols in Plasma by UPLC-MS/MS
作  者:
ZHANG Xue-song;WANG Yu-fei;WANG Guo-dong;XIANG Xue-song;WANG Zhu;Nation Institute for Nutrition and Health Chinese Center for Disease Control and Prevention;Bao' an Central Hospital of Shenzhen;
关键词:
alkylresorcinols;;whole-grain wheat food;;plasma;;UPLC-MS/MS
摘  要:
【Objective】To establish a method for the determination of 2 alkylresorcinols as biomarkers of whole-grain wheat foods by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry(UPLC-MS/MS). 【Method】Internal standard was added in plasma,the ARs was extracted by acetone,the extraction was filtrated and dried under nitrogen,and then dissolved in isopropanol for analysis. The analysis was performed on a cortecs column(2. 1 mm × 100 mm,1. 6μm) and isocratic elution using isopropanol∶acetonitrile =30∶70 as the mobile phase. The samples were determined by mass spectrometry in the negative ion mode with the multiple reaction monitoring mode,quantified by the internal standard method. 【Result】Totally 2 alkylresorcinols had good linearity in the concentration range of 2 ~ 200 ng/mL,r~2> 0. 998 0. The limits of detection for 2 alkylresorcinols was 0. 1 ng/mL,the limits of quantification was 0. 3 ng/mL. Recoveries at 3 different levels were in ranges of 88. 2% ~ 110%,and the relative standard deviations were in ranges of 2. 48% ~ 13. 2%(n = 6). 【Conclusion】This method is accurate and sensitive,the preparation is simple and rapid,which can be used for determination of 2 alkylresorcinols in plasma effectively.

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