卷烟主流烟气总粒相物中挥发性和半挥发性有机酸的分析

采用二氯甲烷萃取、N,O-双(三甲基硅基)三氟乙酰胺硅烷化、反-2-己烯酸和肉桂酸作内标,接预分离柱和选择离子检测GC/MS法同时测定了卷烟主流烟气中的甲酸、乙酸和二十酸等30种有机酸。方法的回收率为74.3%～101.8%,RSD均小于10%。并采用该法测定了10个牌号国产烤烟型卷烟烟气中有机酸含量。该法适于批量卷烟主流烟气总粒相物中挥发性和半挥发性有机酸的快速分析。  

气相色谱-质谱法测定生姜中丙炔氟草胺残留量

本文建立了生姜中丙炔氟草胺残留量的分析方法.试样经乙腈提取,活性炭柱净化,目标农药采用气相色谱-质谱/选择离子监测法（GC-MS/SIM）进行定性、定量分析,方法检出限为0.006mg/kg,在0.02、0.04、0.05、0.1、0.2mg/kg添加水平回收率为62%～105%,相对标准偏差（RSD）5.2%～18%.  

固相萃取气相色谱-质谱联用法测定动物组织中的莱克多巴胺

通过液液分配和固相萃取提取、净化动物组织中添加的莱克多巴胺，TMS衍生化试剂BSTFA（N，O-双（三甲基硅烷基）三氟乙酰胺）衍生化，气相色谱-质谱联用（选择离子模式，选择离子为m/z163、m／z192、m／z234、m／z250）对衍生物检测分析，确定了动物组织中莱克多巴胺的定性、定量分析方法，该法检出限为0．5μg／L，衍生物的峰面积与样品浓度在1～1000μg／L范围内呈良好的线性关系，线性回归系数为0．9998。不同组织中不蚓莱克多巴胺加入量的加标回收率分别为：肝脏70．2％-75．4％，脂肪71．2％-84．7％，肾脏72．8％-80．9％，肌肉75．2％-86．4％；相对标准偏差为1．8％-5．6％。  

黄瓜中噻嗪酮、三唑酮残留量的测定

利用气相色谱-质谱(GC-MS)，电子轰击(EI)法同时测定了黄瓜中噻嗪酮、三唑酮残留量。试样经丙酮-石油醚提取，二氯甲烷萃取，无水硫酸钠干燥，浓缩。选择灵敏度高、干扰少的检测离子，用选择离子监测(SIM)方式测定了其中两种农药残留。噻嗪酮，三唑酮的检出限量分别为0．13和0.013mg／kg，标准添加(0．013-1mg／kg)的回收率为71．1％～123％，测定的相对标准偏差(RSD)为3、4％～17％。  

顶空进样气相色谱质谱法同时检测食品包装材料中的10种残留溶剂

目的 建立顶空气相色谱-质谱检测食品包装材料中10种残留有机溶剂的分析方法。方法 采用GC-MS选择离子监测(SIM)模式进行定量分析。结果 10种溶剂在0.001~0.1 mg/m2浓度范围线性关系良好, 相关系数在0.9999~1.0000, 对最低浓度点进行了重现性实验, RSD均小于10%, 回收率79.0%~106.2%, 精密度1.08％~8.02％。结论 此方法快速、准确可以满足国内外对食品包装材料中10种残留有机溶剂的同时检测。  

固相萃取气相色谱-质谱联用法测定牛奶中的雌三醇

通过液液萃取和固相萃取提取、净化牛奶中添加的雌三醇，TMS衍生化试剂BSTFA衍生化。气相色谱-质谱联用（选择离子模式，选择离子为m／z311，m／z345，m／z414，m／zS04）对衍生物检测分析。确定了牛奶中雌三醇的定性、定量分析方法．该法栓出限为0．5μg／L，衍生物的峰面积与样品质量浓度在1—1000μg／L内呈良好的线性关系，线性回归系数为0．999。不同雌三醇加入量的加标回收率分别为78．2％-86．7％，变异系数为3．2％-3．6％。  

烟草中游离植物甾醇的GC/MS/SIM分析

建立了一种采用二氯甲烷提取、微孔滤膜过滤、气相色谱/质谱/选择离子监测(GC/MS/SIM)定量测定烟草中游离植物甾醇的方法,并采用该法测定了部分烟叶样品、霉变烟叶和部分卷烟样品中的游离植物甾醇含量。结果表明:①该法的检测限为5.12~8.43ng/g,回收率在93%~103%之间,RSD<6%;②香料烟的麦角甾醇含量最高,其次是烤烟,白肋烟最低;③卷烟烟丝中的游离植物甾醇含量与其烟气中苯并[a]芘的释放量呈显著正相关。结论:该法适合批量烟叶样品中甾醇的定量分析。  

Optimization of gas chromatography–single quadrupole mass spectrometry conditions for multiresidue analysis of pesticides in grapes in compliance to EU-MRLs

A single quadrupole GC–MS method was optimized for multiresidue determination of 47 pesticides in grapes with limit of quantifications of each compound in compliance with the EU-MRL requirements. Sample preparation involved extraction of 10 g sample with 10 ml ethyl acetate (+10 g sodium sulphate) by homogenization at 15,000 rpm followed by centrifugation at 3000 rpm. The supernatant was cleaned by dispersive solid phase extraction with primary secondary amine and acidified with 0.1% formic acid. Residues were estimated in selected ion monitoring mode with programmable temperature vaporizer-large volume injection (8 μl). All the GC and MS parameters were thoroughly optimized to achieve satisfactory linearity (R² > 0.99) within 0.01–0.25 mg kg⁻¹ with minimum matrix interferences. Recoveries at 0.01 and 0.02 mg kg⁻¹ were within 67–120% with associated precision RSD below 19%. The method was successfully applied for analysis of the real world samples for incurred residues.  

Production of dipeptidyl peptidase IV inhibitory peptides from defatted rice bran

The insulinotropic hormone glucagon-like peptide-1 is metabolised extremely rapidly by the ubiquitous enzyme dipeptidyl peptidase IV (DPP-IV). Therefore, human DPP-IV is a key regulator involved in the prevention and treatment of type 2 diabetes. To simplify the method of producing an inhibitory peptide against DPP-IV, we focused on rice bran (RB) as a source and subjected proteins from defatted RB to enzymatic proteolysis using 2 commercial enzymes. The RB peptides produced with Umamizyme G exhibited 10 times the inhibitory activity as those produced with Bioprase SP. The half-maximal inhibitory concentration (IC₅₀) value of the RB peptides was 2.3 ± 0.1 mg/ml. Leu-Pro and Ile-Pro were identified as the inhibitory peptides among the RB peptides produced with Umamizyme G. Ile-Pro was the strongest DPP-IV inhibitor among the 15 Xaa-Pro dipeptides and Pro-Ile tested. Ile-Pro competitively inhibited DPP-IV (K_i = 0.11 mM). Mass spectrometry indicated that the contents of Leu-Pro and Ile-Pro in the RB peptides were 2.91 ± 0.52 μg/mg.  

气相色谱-质谱法检测减肥食品中芬氟拉明和西布曲明

采用气相色诲质谱（GC-MS）分析技术，选择离子检测法（SIM），建立了减肥食品中芬氟拉明和西布曲明的测定方法。样品经乙醇超声提取，用HP-5MS石英毛细管柱分离，选择m／z72、114和159用于SIM检测，并恨据提取离子色谱图的峰面积比进行目标物确证，实现了色谱保留时间、质谱特征离子同时定性，消除了减肥食品中复杂基体的干扰，避免了假阳性结果的出现。西布曲明和芬氟拉明在0．1mg／L-50mg／L浓度范围内与峰面积之间线性关系良好，在低、中、高3个添加水平范围内的平均回收率为93．8％曲7．6％，检测限可以达到1．0mg／kg，可用于减肥食品中非法添加芬氟拉明和西布曲明的检测。