目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,...目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,气相色谱-质谱联用仪多反应监测(multiple reaction monitoring,MRM)模式检测,采用基质匹配标准溶液内标法定量。结果218种农药在5~200 ng/mL范围内线性关系良好,相关系数均大于0.995,在0.05、0.10、0.50 mg/kg 3个添加水平的回收率为63.3%~119.9%,相对标准偏差(relative standard deviations,RSDs)为0.78%~18.10%,定量限(limits of the quantitation,LOQs)为10~20μg/kg。结论该方法前处理简单、高效,灵敏度、准确度和精密度高,能满足玉米油中218种农药多残留的分析要求。展开更多
目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测...目的 建立一种Qu ECh ERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定蜂房及其制剂中10种真菌毒素的检测方法。方法 样品经80%乙腈水溶液提取,Qu ECh ERS EMRLipid净化,采用UPLC-MS/MS,在多反应监测(MRM)模式下进行测定,内标法定量。结果 10种真菌毒素含量在各自质量浓度范围内具有较好的线性关系(r>0.999),目标化合物在低、中、高3个质量浓度下的平均回收率为83.8%~107.1%(RSD<6.5%),定量限(LOQ)为0.18~129μg/kg。结论 该法前处理步骤简便,净化效果良好,提高了样品检测效率,内标法定量精准可靠,适用于蜂房及其制剂中10种真菌毒素的同时检测。展开更多
[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established acc...[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established according to Agilent Bond Elut enhanced lipid removal EMR-Lipid technology. [ Methods] Egg was extracted by acidified acetonitrile, purified by Bond Elut EMR-Lipid QuEChERS, and detected by HPLC-MS/MS. [ Results] The three kinds of polyether residues had good linear relationships in the range of 2.0 - 100 μg/L with peak areas, r 〉 0. 999. The recoveries ranged from 84.6% to 107.0%. [ Conclusions ] The method is convenient and accurate, and the quantitative results are accurate and reproducible. It is suitable for the determination of the three kinds of polyether residues in eggs.展开更多
提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟...提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟庚烷磺酸、全氟辛烷磺酸等15种全氟化合物含量的方法。鸡蛋样品(2 g)中加入0.1 mL 20.0μg·L^(-1)同位素内标混合溶液,经10 mL 80%(体积分数)乙腈溶液振荡和超声提取后,离心;分取5 mL滤液,直接过滤过型Captive EMR-Lipid柱净化,收集流出液,氮吹至近干,加入500μL甲醇复溶,经涡旋、离心处理后测定。采用Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,以不同体积比的2 mmol·L^(-1)乙酸铵溶液和甲醇的混合溶液梯度洗脱,在电喷雾离子源负离子扫描模式下,以多反应监测模式检测,同位素内标法定量。结果表明:15种全氟化合物标准曲线的线性范围均为0.125~20.0μg·L^(-1),测定下限(10S/N)为0.05~0.16μg·kg^(-1);在0.500,4.00,16.0μg·kg^(-1)加标浓度水平下,15种目标物的回收率为78.0%~111%,测定值的相对标准偏差(n=6)为0.87%~14%。展开更多
文摘目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,气相色谱-质谱联用仪多反应监测(multiple reaction monitoring,MRM)模式检测,采用基质匹配标准溶液内标法定量。结果218种农药在5~200 ng/mL范围内线性关系良好,相关系数均大于0.995,在0.05、0.10、0.50 mg/kg 3个添加水平的回收率为63.3%~119.9%,相对标准偏差(relative standard deviations,RSDs)为0.78%~18.10%,定量限(limits of the quantitation,LOQs)为10~20μg/kg。结论该方法前处理简单、高效,灵敏度、准确度和精密度高,能满足玉米油中218种农药多残留的分析要求。
基金Supported by Science and Technology Planning Project of Huizhou City(20161117141959)
文摘[Objectives] This study was conducted to establish an LC-MS/MS method for the determination of three kinds of polyether residues in eggs with QuEChERS dSPE EMR-Lipid as a pretreatment method, which was established according to Agilent Bond Elut enhanced lipid removal EMR-Lipid technology. [ Methods] Egg was extracted by acidified acetonitrile, purified by Bond Elut EMR-Lipid QuEChERS, and detected by HPLC-MS/MS. [ Results] The three kinds of polyether residues had good linear relationships in the range of 2.0 - 100 μg/L with peak areas, r 〉 0. 999. The recoveries ranged from 84.6% to 107.0%. [ Conclusions ] The method is convenient and accurate, and the quantitative results are accurate and reproducible. It is suitable for the determination of the three kinds of polyether residues in eggs.
文摘提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟庚烷磺酸、全氟辛烷磺酸等15种全氟化合物含量的方法。鸡蛋样品(2 g)中加入0.1 mL 20.0μg·L^(-1)同位素内标混合溶液,经10 mL 80%(体积分数)乙腈溶液振荡和超声提取后,离心;分取5 mL滤液,直接过滤过型Captive EMR-Lipid柱净化,收集流出液,氮吹至近干,加入500μL甲醇复溶,经涡旋、离心处理后测定。采用Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,以不同体积比的2 mmol·L^(-1)乙酸铵溶液和甲醇的混合溶液梯度洗脱,在电喷雾离子源负离子扫描模式下,以多反应监测模式检测,同位素内标法定量。结果表明:15种全氟化合物标准曲线的线性范围均为0.125~20.0μg·L^(-1),测定下限(10S/N)为0.05~0.16μg·kg^(-1);在0.500,4.00,16.0μg·kg^(-1)加标浓度水平下,15种目标物的回收率为78.0%~111%,测定值的相对标准偏差(n=6)为0.87%~14%。
