蔬菜和水果中杀菌剂的高效液相色谱-串联质谱检测法
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摘要
目的建立高效液相色谱-串联质谱(LC-MS/MS)法定量测定蔬菜和水果中11种杀菌剂的方法。方法样品以快速样品前处理技术(Qu ECh ERS法)净化,经LC-MS/MS检测,以选择离子扫描(SIM)模式检测目标化合物的特征离子进行定性定量分析。结果 11种杀菌剂在测定的范围内线性关系良好(r>0.999 0),方法的检出限为0.4~2.5μg/kg(S/N=3)。在加标水平为40、60、80μg/L时,方法的回收率为75.6%~108.2%,相对标准偏差为1.2%~7.5%。结论该方法前处理简单,分析时间短、选择性好和灵敏度高,适用于蔬菜和水果中杀菌剂的检测。
[Objective]To establish the high performance liquid chromatography tandem mass spectrometry(LC-MS/MS) method for quantitative determination of 11 microbicides in vegetables and fruits. [Methods] The samples were purified by Qu ECh ERS,detected by LC-MS/MS. The characteristic ions of target compound were qualitatively and quantitatively analyzed by LC-MS/MS under SIM mode. [Results] Within the range, the linear relation of 11 microbicides was well(r>0.999 0), and the detection limits were 0.4-2.5 μg/kg(S/N=3). When the standard addition levels were 40, 60 and 80 μg/L, the recovery rates were 75.6%-108.2%,and the RSD were 1.2%-7.5%. [Conclusion] This method has the advantages of simple pretreatment, short analysis time, good selectivity and high sensitivity, which is suitable for the determination of microbicides in vegetables and fruits.
[Objective]To establish the high performance liquid chromatography tandem mass spectrometry(LC-MS/MS) method for quantitative determination of 11 microbicides in vegetables and fruits. [Methods] The samples were purified by Qu ECh ERS,detected by LC-MS/MS. The characteristic ions of target compound were qualitatively and quantitatively analyzed by LC-MS/MS under SIM mode. [Results] Within the range, the linear relation of 11 microbicides was well(r>0.999 0), and the detection limits were 0.4-2.5 μg/kg(S/N=3). When the standard addition levels were 40, 60 and 80 μg/L, the recovery rates were 75.6%-108.2%,and the RSD were 1.2%-7.5%. [Conclusion] This method has the advantages of simple pretreatment, short analysis time, good selectivity and high sensitivity, which is suitable for the determination of microbicides in vegetables and fruits.
引文
[1]于功昌,王筱芬.苯并咪唑杀菌剂的雄性生殖毒性作用机制研究进展[J].职业与健康,2014,30(18):2661-2663,2669.
[2]中华人民共和国卫生和计划生育委员会,中华人民共和国农业部.食品安全国家标准食品中农药最大残留限量:GB 2763-2014[S].北京:中国标准出版社,2014.
[3]许泳吉,刘云云,韩玮,等.固相萃取-高效液相色谱法同时测定烟草中吡虫啉和多菌灵[J].青岛科技大学学报(自然科学版),2016,26(1):26-31.
[4]苑学霞,梁京芸,王文博,等.苹果和土壤中甲基硫菌灵及其代谢物残留消解动态[J].生态环境学报,2016,42(1):135-140.
[5]东保柱,王振,景岚,等.HPLC法同时检测土壤中多菌灵、菌核净、速克灵、咪鲜胺4种杀菌剂[J].农药,2016,3(3):205-207.
[6]秦曙,乔雄梧,王霞,等.气相色谱法检测22种基质中的4种二硫代氨基甲酸盐类农药残留[J].色谱,2010,28(12):1162-1167.
[7]乙小娟,王玥,孙建刚,等.气质联用法检测豆芽中的百菌清残留量[J].分析试验室,2010,7(1):379-381.
[8]程盛华,杨春亮,曾绍东,等.分散固相萃取-超高效液相色谱-串质普法测定豆芽中10种植物生长剂和杀菌剂[J].食品工业科技,2016,37(12):53-59.
[9]黄志波,昊春梅,李敬钊,等.固相萃取超高效液相色谱质谱/质谱法同时测定蔬菜中7种杀菌剂的残留量[J].广东农业科学,2011,24(5):80-83.
[10]钟冬莲,刘毅华,沈丹玉,等.固相萃取-液相色谱-电喷雾串联质谱法测定鲜枣中14种农药残留[J].食品与生物技术学报,2015,34(7):731-737.
[11]王炼,朱作芳,羊雨婷.同位素内标-液相色谱-串联质谱法测定水果中11种农药残留量[J].中国食品卫生杂志,2016,28(2):209-213.
[12]许欣欣,陈慧玲,毛丽莎,等.蔬菜和水果中多菌灵的Qu ECh ERS前处理高效液相色谱检测法[J].职业与健康,2013,29(18):2312-2314.
[13]孔璇,申雷,郑党儿.液相色谱-串联质谱法测定黄瓜中多菌灵含量的测量不确定度评定[J].职业与健康,2015,31(24):3411-3416.
[14]孙亚米,吕燕,吴银良.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,36(12):230-236.
[15]魏畅,傅红,郑俊超,等.Qu ECHERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].中国食品学报,2016,16(11):189-194.
[2]中华人民共和国卫生和计划生育委员会,中华人民共和国农业部.食品安全国家标准食品中农药最大残留限量:GB 2763-2014[S].北京:中国标准出版社,2014.
[3]许泳吉,刘云云,韩玮,等.固相萃取-高效液相色谱法同时测定烟草中吡虫啉和多菌灵[J].青岛科技大学学报(自然科学版),2016,26(1):26-31.
[4]苑学霞,梁京芸,王文博,等.苹果和土壤中甲基硫菌灵及其代谢物残留消解动态[J].生态环境学报,2016,42(1):135-140.
[5]东保柱,王振,景岚,等.HPLC法同时检测土壤中多菌灵、菌核净、速克灵、咪鲜胺4种杀菌剂[J].农药,2016,3(3):205-207.
[6]秦曙,乔雄梧,王霞,等.气相色谱法检测22种基质中的4种二硫代氨基甲酸盐类农药残留[J].色谱,2010,28(12):1162-1167.
[7]乙小娟,王玥,孙建刚,等.气质联用法检测豆芽中的百菌清残留量[J].分析试验室,2010,7(1):379-381.
[8]程盛华,杨春亮,曾绍东,等.分散固相萃取-超高效液相色谱-串质普法测定豆芽中10种植物生长剂和杀菌剂[J].食品工业科技,2016,37(12):53-59.
[9]黄志波,昊春梅,李敬钊,等.固相萃取超高效液相色谱质谱/质谱法同时测定蔬菜中7种杀菌剂的残留量[J].广东农业科学,2011,24(5):80-83.
[10]钟冬莲,刘毅华,沈丹玉,等.固相萃取-液相色谱-电喷雾串联质谱法测定鲜枣中14种农药残留[J].食品与生物技术学报,2015,34(7):731-737.
[11]王炼,朱作芳,羊雨婷.同位素内标-液相色谱-串联质谱法测定水果中11种农药残留量[J].中国食品卫生杂志,2016,28(2):209-213.
[12]许欣欣,陈慧玲,毛丽莎,等.蔬菜和水果中多菌灵的Qu ECh ERS前处理高效液相色谱检测法[J].职业与健康,2013,29(18):2312-2314.
[13]孔璇,申雷,郑党儿.液相色谱-串联质谱法测定黄瓜中多菌灵含量的测量不确定度评定[J].职业与健康,2015,31(24):3411-3416.
[14]孙亚米,吕燕,吴银良.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,36(12):230-236.
[15]魏畅,傅红,郑俊超,等.Qu ECHERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].中国食品学报,2016,16(11):189-194.