基于HS-SPME-GC-MS的青梅酒香气成分研究

[目的]为更好地勾兑青梅酒,研究青梅浸泡酒、青梅汁、青梅汁发酵酒以及浸泡基酒的香气成分.[方法]采用顶空固相微萃取(HS-SPME)与气相色谱质谱(GC-MS)相结合的方法定性分析浸泡基酒、青梅浸泡酒、青梅汁及青梅汁发酵酒4种样品的香气成分.[结果]试验显示,4个样品依次检测出14、32、17、46种香气成分,香气成分本质的差异决定了其特有的风味和口感.其中,青梅在浸泡过程中产生的特有香气成分为苯甲醛、S-(-)-2-甲基-1-丁醇、苯甲酸乙酯、5-羟甲基糠醛等.青梅汁中特有的香气成分为糠醛、苯乙醇、苯甲醇等.青梅汁发酵酒中产生的主要微量香气成分有苯乙醇(6.941％,峰面积相对百分含量,下同)、异戊醇(6.940％)、辛酸乙酯(3.734％)、癸酸乙酯(2.590％)、己酸乙酯(2.479％)、9-癸烯酸乙酯(2.080％)、5-羟甲基糠醛(1.756％)等.[结论]研究可为青梅酒的品质改善提供科学依据和数据参考.     

不同贮藏时间的普洱茶香气成分分析

采用顶空—固相微萃取技术提取不同贮藏时间的普洱茶香气成分, 经气质联用分析鉴定, 结果表明, 贮藏30 年、25 年、6 年和当年生产的茶样中, 萜烯化合物及其衍生物含量分别为51.42%、89.15%、74.10%、39.72%。但陈茶与新茶中的萜烯化合物及其衍生物的种类却有明显的不同, 陈茶中以反-丁香烯为主, 在贮藏30年、25年、6年茶样中的含量分别达36.78%、66.98%、56.08% , 而当年生产的样品以愈创木烯为主, 其含量达33130% , 反- 丁香烯含量仅为1102%。与当年生产的茶样相比, 陈茶香气成分种类和含量都较少, 贮藏30年、25年、6年茶样分别鉴定出23、24、22种香气化合物, 而当年生产的茶样共鉴定出36种化合物。     

解淀粉芽孢杆菌B9601-Y2对玉米挥发物质的影响

为了明确解淀粉芽孢杆菌B9601-Y2(简称Y2)防病机制,利用顶空抽提法收集Y2菌液和喷施Y2后玉米幼苗挥发物,并通过气相色谱-质谱联用仪对其进行分离和鉴定,共收集到18种Y2菌液挥发物和42种玉米活体植株挥发物。玉米释放醛类化合物8种、萜烯类11种,庚醛、十二烷、癸醛和十三烷为菌液和玉米植株共同抽提到的挥发物。不同处理收集的玉米活体植株挥发物组分种类和相对含量存在差异,Y2处理玉米1、3和5 d后,玉米新出现了1-乙基-2-甲基环戊烷、2-辛烯醛、十一烷、十四碳烯和β-愈创木烯5种化合物,α-衣兰烯等11种化合物相对含量极显著地提高,芳樟醇等8种化合物出现振荡,反-罗勒烯等6种化合物消失;喷施菌液7 d后,Y2对玉米活体植株挥发物种类与相对含量都恢复到常态。     

不同类型梅花品种及近缘种山桃挥发性成分分析

[目的]研究不同类型梅花品种及山桃花朵挥发性成分的差异。[方法]采用顶空-固相微萃取与气相色谱-质谱联用技术对梅花品种青岛朱砂、黑美人、丰后、淡丰后、燕杏梅和山桃花朵挥发性成分进行分析。[结果]从几种植物中共鉴定出20种挥发物。不同类型梅花品种及山桃植物花朵挥发物数量和含量有很大的变化,苯基/苯丙烷类芳香族的化合物含量占有绝对的优势,其中苯甲醛、苯甲醇和乙酸苯甲酯等是梅花及山桃花朵挥发物的主要成分,出现的频率高达100%。[结论]为开发利用梅花香气资源和花香育种提供了科学依据。     

蒜薹挥发性风味成分顶空取样GC-MS 分析

采用顶空取样结合GC-MS 对蒜薹的挥发性风味成分进行了分析,结果表明,蒜薹中含有
23 种挥发性成分,其中含硫化合物15 种,相对含量为99.42%,主要成分为二烯丙基二硫醚（66.52%）、
1,3-二噻烷（15.44%）、二烯丙基三硫醚（7.15%）、二甲基二硫醚（1.24%）、二烯丙基硫醚（1.09%）和
2-烯丙基甲基三硫醚（2.66%）等6 种;与水蒸气蒸馏法相比,顶空取样检出的含硫化合物虽然种类少,
但相对含量高,且硫醚、多噻烷和硫代环己烯3 类主要成分都有检出。     

饲用调味剂稳定性的评价与研究

本文阐述了通过冷冻聚焦顶空累积进样毛细管气相色谱评价调味剂稳定性的方法,并针对调味剂应用中大家所关切的问题,对市售仔猪调味剂加入饲料后自然贮放和制粒温度下加热不同时间“香气”的衰减情况进行了实际研究与探讨,分析了影响调味剂稳定性的主要因素及产品开发应用中应注意的问题。文章还结合动物偏好试验,得出了一些具有参考意义的结果。     

饲料调味剂载体的吸附强度测定方法探讨

阐述了饲料调味剂载体的吸附作用的测定方法。采用顶空气体色谱法，以乳酸乙酯为标记，比较容易地测得所有载体的吸附强度。利用此法，测得常见载体的吸附强度的大小顺序为活性炭＞海泡石粉＞淀粉＞玉米粉＞二氧化硅＞碳酸钙。     

Feasibility of measuring dissolved carbon dioxide based on head space partial pressures

We describe an instrument prototype that measures dissolved carbon dioxide (DC) without need for standard wetted probe membranes or titration. DC is calculated using Henry’s Law, water temperature, and the steady-state partial pressure of carbon dioxide that develops within the instrument’s vertical gas–liquid contacting chamber. Gas-phase partial pressures were determined with either an infrared detector (ID) or by measuring voltage developed by a pH electrode immersed in an isolated sodium carbonate solution (SC) sparged with recirculated head space gas. Calculated DC concentrations were compared with those obtained by titration over a range of DC (2, 4, 8, 12, 16, 20, 24, and 28 mg/l), total alkalinity (35, 120, and 250 mg/l as CaCO₃), total dissolved gas pressure (−178 to 120 mmHg), and dissolved oxygen concentrations (7, 14, and 18 mg/l). Statistically significant (P<0.001) correlations were established between head space (ID) and titrimetrically determined DC concentrations (R²=0.987–0.999, N=96). Millivolt and titrimetric values from the SC solution tests were also correlated (P<0.001, R²=0.997, N=16). The absolute and relative error associated with the use of the ID and SC solution averaged 0.9 mg/l DC and 7.0% and 0.6 mg/l DC and 9.6%, respectively. The precision of DC estimates established in a second test series was good; coefficients of variation (100(SD/mean)) for the head space (ID) and titration analyses were 0.99% and 1.7%. Precision of the SC solution method was 1.3%. In a third test series, a single ID was coupled with four replicate head space units so as to permit sequential monitoring (15 min intervals) of a common water source. Here, appropriate gas samples were secured using a series of solenoid valves (1.6 mm bore) activated by a time-based controller. This system configuration reduced the capital cost per sample site from US$ 2695 to 876. Absolute error averaged 2.9, 3.1, 3.7, and 2.7 mg/l for replicates 1–4 (N=36) during a 21-day test period (DC range, 36–40 mg/l). The ID meter was then modified so as to provide for DO as well as DC measurements across components of an intensive fish production system.     

Identification and quantitative determination of 2-acetyl-1-pyrroline using GC-TOF MS combined with HS and HS-SPME pretreatment

2-Acetyl-1-pyrroline (2-AP) was recognized as the key characteristic volatile in aromatic rice. In this paper, two precise and rapid methods for quantitative determination of 2-AP by headspace-gas chromatography-time-of-flight mass spectrometry (HS-GC-TOF MS) and headspace-solid phase micro-extraction-gas chromatography-time-of-flight mass spectrometry (HS-SPME-GC-TOF MS) have been presented and compared. Chromatograms of 2-AP and internal standard (2-methyl-3-heptanone) in samples were extracted by accurate masses, and the response ratios of 2-AP to internal standard were used for constructing matrix-matched standard curve with the blanks deducted. Pretreatment conditions such as temperature and extractant amount were optimized. Linear ranges of two methods were 1–150 ng g⁻¹ with linear correlation coefficients (r) of 0.9998 and 0.9997, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) of HS-GC-TOF MS method were 0.68 ng g⁻¹ and 2.27 ng g⁻¹. LOD and LOQ of HS-SPME-GC-TOF MS method were 0.46 ng g⁻¹ and 1.50 ng g⁻¹, and could be reduced to 0.02 ng g⁻¹ and 0.06 ng g⁻¹, respectively, in the case of splitless mode. At spiking level of 100 ng g⁻¹, recoveries were 94.19–116.00% and 95.57–107.49% for HS-GC-TOF MS method and HS-SPME-GC-TOF MS method, respectively.