超高效液相色谱-串联质谱法快速测定植物油中黄曲霉毒素B_1
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摘要
2.500g植物油样品用10 mL甲醇(7+3)溶液提取,以6 000r·min~(-1)转速离心10min,在-20℃冷冻30min后,上清液经0.22μm有机滤膜过滤,采用超高效液相色谱-串联质谱法快速测定滤液中黄曲霉毒素B_1的含量。以Accucore aQ色谱柱为固定相,以不同体积比的含5mmol·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正离子源和选择离子监测模式。黄曲霉毒素B_1的质量浓度在0.50～10.00μg·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.02μg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为86.0%～96.6%,回收量的相对标准偏差(n=6)为5.6%～8.4%。
The vegetable oil sample(2.500 g) was extracted with 10 mL of methanol(7+3) solution and then centrifugated for 10 min at the speed of 6 000 r·min~(-1).After freezing for 30 min at -20℃,the supernatant was filtered with 0.22μm organic filter membrane.UHPLC-MS/MS was applied to the rapid determination of aflatoxin B_1 in the filtrate.Accucore aQ chromatographic column 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 the selected ion monitoring mode were adopted in MS/MS.Linear relationship between values of peak area and mass concentration of aflatoxin B_1 was kept in the range of 0.50-10.00μg·L~(-1),with detection limit(3S/N) of 0.02μg·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 86.0%-96.6%,with RSDs(n=6) of recovery amounts in the range of 5.6%-8.4%.
The vegetable oil sample(2.500 g) was extracted with 10 mL of methanol(7+3) solution and then centrifugated for 10 min at the speed of 6 000 r·min~(-1).After freezing for 30 min at -20℃,the supernatant was filtered with 0.22μm organic filter membrane.UHPLC-MS/MS was applied to the rapid determination of aflatoxin B_1 in the filtrate.Accucore aQ chromatographic column 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 the selected ion monitoring mode were adopted in MS/MS.Linear relationship between values of peak area and mass concentration of aflatoxin B_1 was kept in the range of 0.50-10.00μg·L~(-1),with detection limit(3S/N) of 0.02μg·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 86.0%-96.6%,with RSDs(n=6) of recovery amounts in the range of 5.6%-8.4%.
引文
[1]吴坤,李存雄,姜金仲,等.UPLC-MS/MS法测定花生油中黄曲霉毒素B1的含量[J].食品研究与开发,2016,37(14):111-115.
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[5] GB 2761-2017食品安全国家标准食品中真菌毒素限量[S].
[6] GB 5009.22-2016食品安全国家标准食品中黄曲霉毒素B族和G族的测定[S].
[7]鲍蕾,包振民,吕宁,等.中国出口花生黄曲霉毒素检测能力验证研究[J].食品科学,2009,30(24):381-384.
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[9]侯磊磊,柴梅梅,米林锋,等.高效液相色谱-柱后光化学衍生法测定油茶中黄曲霉毒素B1的方法研究[J].食品安全质量检测学报,2018,9(11):2631-2635.
[10]赵浩军,王坤,杨卫花,等.高效液相色谱柱后光化学反应-荧光检测茶叶中黄曲霉毒素B1[J].茶叶科学,2013,33(3):237-241.
[11]竺巧玲,俞薇,楼乔明.植物油黄曲霉毒素B1含量的检测及能力验证[J].食品工业,2015,36(2):274-277.
[12]王岩松,范世华,李华锋,等.固相萃取-高效液相色谱/串联质谱检测谷物中黄曲霉毒素B1、B2、G1、G2和M1[J].分析试验室,2011,30(10):63-67.
[13]宫小明,任一平,董静,等.超高效液相色谱串联质谱法测定花生、粮油中18种真菌毒素[J].分析测试学报,2011,30(1):6-12.
[14]程盛华,杨春亮,曾绍东,等.QuEChERS-超高效液相色谱-串联质谱法测定植物油中黄曲霉毒素[J].化学试剂,2015,37(10):897-902.
[15]刘妍,陈坚,谭贵良,等.QuEChERS-超高效液相色谱串联质谱法测定发酵黑茶中的10种真菌毒素[J].现代食品科技,2017,33(7):280-288.
[2]郝莉花,陈复生.免疫亲和柱净化-UPLC-MS/MS测定花生中黄曲霉毒素B1[J].食品工业,2017,38(1):269-272.
[3]康绍英,周兴旺,张继红,等.液相色谱-串联质谱法同时检测食品中的4种黄曲霉毒素[J].食品与机械,2013,29(2):77-81.
[4]王浩,杨红梅,郭启雷,等.高效液相色谱-串联质谱法同时测定植物油中苯并芘与黄曲霉毒素B1,B2,G1,G2[J].分析测试学报,2014,33(8):911-916.
[5] GB 2761-2017食品安全国家标准食品中真菌毒素限量[S].
[6] GB 5009.22-2016食品安全国家标准食品中黄曲霉毒素B族和G族的测定[S].
[7]鲍蕾,包振民,吕宁,等.中国出口花生黄曲霉毒素检测能力验证研究[J].食品科学,2009,30(24):381-384.
[8]庞世琦,刘青,奚星林,等.花生油中黄曲霉毒素B1检测能力验证研究[J].中国食品卫生杂志,2013,25(2):169-173.
[9]侯磊磊,柴梅梅,米林锋,等.高效液相色谱-柱后光化学衍生法测定油茶中黄曲霉毒素B1的方法研究[J].食品安全质量检测学报,2018,9(11):2631-2635.
[10]赵浩军,王坤,杨卫花,等.高效液相色谱柱后光化学反应-荧光检测茶叶中黄曲霉毒素B1[J].茶叶科学,2013,33(3):237-241.
[11]竺巧玲,俞薇,楼乔明.植物油黄曲霉毒素B1含量的检测及能力验证[J].食品工业,2015,36(2):274-277.
[12]王岩松,范世华,李华锋,等.固相萃取-高效液相色谱/串联质谱检测谷物中黄曲霉毒素B1、B2、G1、G2和M1[J].分析试验室,2011,30(10):63-67.
[13]宫小明,任一平,董静,等.超高效液相色谱串联质谱法测定花生、粮油中18种真菌毒素[J].分析测试学报,2011,30(1):6-12.
[14]程盛华,杨春亮,曾绍东,等.QuEChERS-超高效液相色谱-串联质谱法测定植物油中黄曲霉毒素[J].化学试剂,2015,37(10):897-902.
[15]刘妍,陈坚,谭贵良,等.QuEChERS-超高效液相色谱串联质谱法测定发酵黑茶中的10种真菌毒素[J].现代食品科技,2017,33(7):280-288.