HPLC-MS/MS Determination of Aflatoxins and Their Homologues in Supplementary Cookies for Infants and Young Children
摘 要
粉碎的婴幼儿辅助饼干食品样品经体积比为89:10:1的乙腈-水-乙酸混合液提取,采用净化剂为50 mg十八烷基硅烷、30 mg N-丙基乙二胺和30 mg氨丙基的QuEChERS方法净化,采用高效液相色谱-串联质谱法测定净化液中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、O-甲基柄曲霉素、柄曲霉素、黄曲霉毒素M1、黄曲霉毒素M2等8种黄曲霉毒素及其同系物的含量。以AQ-C18 HP色谱柱(2.1 mm×100 mm,3.0 μm)为固定相,以不同体积比的含5 mmol·L-1乙酸铵的0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正离子扫描模式和多反应监测模式。8种黄曲霉毒素及其同系物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.05~0.10 μg·kg-1,测定下限(10S/N)为0.15~0.30 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为76.3%~95.9%,测定值的相对标准偏差(n=6)为3.1%~11%。
Abstract
The crushed sample of supplementary cookies for infants and young children was extracted with mixture of acetonitrile, water and acetic acid with volume ratio of 89∶10∶1, and purified by QuEChERS method with purification agents of 50 mg ODS, 30 mg PSA and 30 mg NH2. HPLC-MS/MS was applied to the determination of 8 aflatoxins and their homologues, i.e. AFB1, AFB2, AFG1, AFG2, MST, ST, AFM1 and AFM2 in the purified liquid. AQ-C18 HP chromatographic column (2.1 mm×100 mm, 3.0 μm) was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution containing 5 mmol·L-1 ammonium acetate and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 8 aflatoxins and their homologues were kept in definite ranges, with detection limits (3S/N) in the range of 0.05-0.10 μg·kg-1 and lower limits of determination (10S/N) in the range of 0.15-0.30 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 76.3%-95.9%, with RSDs (n=6) of determined values in the range of 3.1%-11%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202005015
所属栏目 专题报道(药物分析)
基金项目 潍坊市科学技术发展计划项目(2018GX056)
收稿日期 2019/12/16
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备注张艾青,讲师,研究方向为食品科学,zhangaiqingwf@163.com
引用该论文: ZHANG Aiqing. HPLC-MS/MS Determination of Aflatoxins and Their Homologues in Supplementary Cookies for Infants and Young Children[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(5): 570~576
张艾青. 高效液相色谱-串联质谱法测定婴幼儿辅助饼干食品中黄曲霉毒素及其同系物[J]. 理化检验-化学分册, 2020, 56(5): 570~576
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参考文献
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【14】韩艺烨,邓年,谢建军,等.酸辅助分散液液微萃取-高效液相色谱-串联质谱法测定果汁中多种真菌毒素[J].分析化学, 2019,47(3):455-462.
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【17】刘丹,韩小敏,李凤琴,等.花生油和玉米油中多组分真菌毒素高效液相色谱-串联质谱检测方法的建立[J].食品科学, 2017,38(10):297-304.
【2】MISHRA H N, DAS C. A review on biological control and metabolism of aflatoxin[J]. Critical Reviews in Food Science and Nutrition, 2003,43(3):245-264.
【3】任贝贝,王可,杨力学,等.液相色谱-串联质谱法检测婴幼儿食品中6种黄曲霉毒素[J].食品安全质量检测学报, 2015,6(10):3863-3870.
【4】DUTTON M F. Enzymes and aflatoxin biosynthesis[J]. Microbiological Reviews, 1988,52(2):274-295.
【5】耿建强,赵丽,张旭,等.我国婴幼儿营养米粉中真菌毒素污染情况调查[J].中国食品卫生杂志, 2017,29(1):67-70.
【6】李颖.一款婴幼儿食品检出黄曲霉素B1[J].中国质量万里行, 2017(9):62-63.
【7】郭礼强,宫小明,孙军,等.高效液相色谱-质谱法同时测定曲霉菌代谢物中的黄曲霉毒素及其同系物[J].分析试验室, 2015,34(6):677-682.
【8】MANKEVICIENÉ A, JABLONSKYTÉ-RAŠCÉ D, MAIKŠTÉNIENÉ S. Occurrence of mycotoxins in spelt and common wheat grain and their products[J]. Food Additives & Contaminants:Part A, 2014,31(1):132-138.
【9】SEWRAM V, SHEPHARD G S, VAN DER MERWE L, et al. Mycotoxin contamination of dietary and medicinal wild plants in the eastern cape Province of south Africa[J]. Journal of Agricultural and Food Chemistry, 2006,54(15):5688-5693.
【10】王桂苓,邢化冰,李琳琳,等.光化学柱后衍生-高效液相色谱法测定婴幼儿营养米粉中的黄曲霉毒素B1[J].化学分析计量, 2014,23(3):28-31.
【11】李毅芳,韩晓,聂晓玲.2013年咸阳市食品化学污染物监测分析[J].中国卫生检验杂志, 2015,25(14):2404-2407.
【12】王韦岗,强敏,端礼钦.复合免疫亲和柱-高效液相色谱法同时测定谷物及其制品中9种真菌毒素[J].色谱, 2018,36(12):1330-1336.
【13】吴宇,叶金,张冰,等.稳定同位素稀释-超高效液相色谱-串联质谱法快速测定植物油中16种真菌毒素[J].分析化学, 2018,46(6):975-984.
【14】韩艺烨,邓年,谢建军,等.酸辅助分散液液微萃取-高效液相色谱-串联质谱法测定果汁中多种真菌毒素[J].分析化学, 2019,47(3):455-462.
【15】熊丽蓓,洪新宇,宋越,等.应用代谢组学方法对细菌培养体中霉菌毒素的研究[J].环境与职业医学, 2009,26(2):140-143.
【16】郑翠梅,张艳,王松雪,等.液相色谱-飞行时间质谱同时测定粮食中13种真菌毒素[J].分析测试学报, 2012,31(4):383-389.
【17】刘丹,韩小敏,李凤琴,等.花生油和玉米油中多组分真菌毒素高效液相色谱-串联质谱检测方法的建立[J].食品科学, 2017,38(10):297-304.
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