建立超高效液相色谱-三重四极杆质谱法同时检测大米基质中8种真菌毒素的方法，对地理标志产品松江大米中真菌毒素的污染情况进行监测。大米样品经提取液乙腈水混合液(84:16，体积比)超声提取后，取部分提取液加入内标溶液，混匀后过多功能净化柱MycoSep229净化，采用Waters Acquity UPLC BEH C18色谱柱(2。1 mm ×50 mm，1。7 μm)，以体积分数0。1％甲酸水溶液-乙腈作为流动相进行梯度洗脱，分离黄曲霉毒素B1(Aflatoxin B1，AFB1)、黄曲霉毒素 B2(Aflatoxin B2，AFB2)、黄曲霉毒素 G1(Aflatoxin G1，AFG1)、黄曲霉毒素 G2(Aflatoxin G2，AFG2)、伏马毒素 B1(Fumonisins B1，FB1)、伏马毒素 B2(Fumonisins B2，FB2)、伏马毒素B3(Fumonisins B3，FB3)、赭曲霉毒素A(Ochratoxin A，OTA)8种真菌毒素化合物，该方法采用电喷雾离子化正离子模式，以多反应监测方式进行。AFB1、AFG1、FB1、FB2、FB3、OTA6种真菌毒素在0。5～15。0 μg/L范围内线性良好，AFB2、AFG2在0。125～3。750 μg/L范围内线性良好，线性相关系数r均大于0。999;8种化合物定量限(limit of quantifications，LOQs)范围为0。01～0。25 μg/kg，比国标中相同方法的定量限降低2～80倍不等;在低、中、高三水平加标，其回收率均在95％～120％范围内，相对标准偏差(relative standard deviations，RSDs)为1。5％～8。9％(N=6)。本方法前处理简单，方法利用率高，结果准确可靠，利用该方法检测的20批新上市松江大米中真菌毒素污染情况比较乐观，对人体的健康危害较低。
Determination of 8 Mycotoxins in Product of Geographical Indication Songjiang Rice by Ultra-high Performance Liquid Chromatography-Mass Spectrometry
To establish a method for the determination of 8 mycotoxins in rice matrix by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS)and monitor the pollution levels of mycotoxins in product of geographical indication Songjiang rice.The rice products were processed with acetonitrile a-queous solution(84:16,volume ratio)by ultrasonic extraction.Parts of the extract were added some internal stand-ard solutions and purified by the Mcosep 229 multifunctional cleanup column.The 8 mycotoxin compounds are sepa-rated by Waters Acquity UPLC BEH C18 column(2.1 mm ×50 mm,1.7 pm)with volume fraction 0.1％formic acid aqueous solution-acetonitrile as mobile phases for gradient elution.They were detected by electrospray ion source in positive mode with multiple reaction monitoring(MRM)mode.The calibration curves showed great lineari-ties in the range of 0.5-15.0 μg/L,such as Aflatoxin B1 and other 5 mycotoxins.The other calibration curves of Aflatoxin B2 and Aflatoxin G2 also showed good linearities in the range of 0.125-3.750 μg/L.The correlation coefficient(r)of the calibration curves of all the compounds were above 0.999.The limits of quantifications(LOQs)of the 8 compounds were in the range of 0.01-0.25 μg/kg,being 2-80 times lower than those of the same methods in the national standards.The recoveries of the 8 compounds at low,medium and high levels could reach 95％-120％,respectively,and the relative standard deviations(RSDs)were 1.5％-8.9％(N=6).In general,the method had the advantages of simple pretreatment,high utilization rate and accurate and reliable results.The pollution situation of mycotoxins in 20 batches of new Songjiang rice in the market deter-mined by the above method was optimistic,and the risk to human health was at a lower level.
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