改良的QuEChERS结合气相色谱-质谱法测定新鲜水果和肉中肉桂醛残留

建立了改良的QuEChERS技术结合气相色谱-质谱检测水果和肉中肉桂醛残留量的定性定量分析方法。试样用乙酸乙酯溶液均质提取,经N-丙基乙二胺（PSA）、石墨化炭黑（GCB）、C₁₈固相吸附剂净化,在电子轰击电离（EI）源、选择离子监测（SIM）模式下检测,外标法定量。肉桂醛在0.01~0.5 mg/L范围内线性关系良好,相关系数大于0.999。水果和鲜肉中肉桂醛的定量限分别为0.5 mg/kg和1.0 mg/kg。在3个添加水平下,肉桂醛的加标回收率为81.9%~104.5%,相对标准偏差（RSD,n=6）为1.1%~8.6%。该方法操作简单,净化效果好,适用于水果和鲜肉中肉桂醛残留量的快速检测。     

Surface-enhanced Raman spectroscopy coupled with gold nanoparticles for rapid detection of amoxicillin residues in duck meat

Antibiotic residues in meat pose serious threats to human beings and animals, and are one of the main food safety concerns all around the world. A novel method based upon surface-enhanced Raman spectroscopy (SERS) coupled with gold nanoparticles was developed in this study for rapid detection of amoxicillin residues in duck meat, one widely used in duck farming. Three different particle sizes of gold nanoparticles were synthesized using 0.3, 0.7, and 1.1?mL 1% trisodium citrate, while 0.7?mL was found to be the optimal volume as Raman enhancement substrate for the detection of amoxicillin residues in duck meat. The amounts of gold nanoparticles (0.5?mL), duck meat extract containing amoxicillin (50?μL), and sodium chloride solution (100?μL), as well as adsorption time (5?min) were optimized by single factor experiments. A calibration curve with the determination coefficient of 0.9661 was established for quantitative analysis of unknown amoxicillin samples. The average recoveries of amoxicillin residues in duck meat extract were 96–139%. This study provided a rapid and simple approach to analyze amoxicillin residues in duck meat in excess of 0.2?mg?L^?1 using SERS coupled with gold nanoparticles, which has the potential for wide applications in the detection of the antibiotic residues in meat.     

圆背角无齿蚌的主要营养成分

分析了取珠后圆背角无齿蚌肉（Ａｎａｔｏｎｔａ　ｗｏｏｄｉａｎａ　ｐａｃｉｆｉｃａ）的营养成分,结果表明：蚌肉的含水量为８１．３５％;干燥后的蚌肉中蛋白质含量为５６．５４％,灰分５．７８％,脂肪３．４８％,糖类３２．１７％,含有丰富的人体必需氨基酸（ＥＡＡ之和占总氨基酸量的３９．７３％）和呈味氨基酸（Ｇｌｕ、Ａｓｐ、Ｇｌｙ等）,此外蚌肉还含有丰富的Ｃａ、Ｐ、Ｆｅ和一定量人体必需的Ｚｎ、Ｃｕ等微量元素．     

腌肉制品发色剂的研究

腌肉制品发色剂历来均用硝盐,但最近发现亚硝基对人体健康有害。我们采用GDL为主作香肠的发色剂,发色效果理想,有一定实用价值。     

五角棱镜光束转向波前误差的分析与检测

从分析五角棱镜的角度制造误差产生的光学平行差入手,建立起五角棱镜的光输出平面波前与运动误差和角度制造误差产生的扫描激光束转向的波前改变量之间的关系.采用渥拉斯顿棱镜型双频激光干涉仪实时测量五角棱镜的运动误差,即可计算出扫描激光束转向的波前误差,以便在大型望远系统波前测量时对此误差加以修正.     

Determination of biogenic amines in fresh and processed meat by suppressed ion chromatography-mass spectrometry using a cation-exchange column

A new method for simultaneous determination of underivatized biogenic amines based on the separation by cation-exchange chromatography and suppressed conductivity coupled with mass spectrometry detection has been developed. The method has been applied to the analysis of cadaverine, putrescine, histamine, agmatine, phenethylamine and spermidine in processed meat products. The amines were extracted from muscle tissue with methanesulfonic acid without any additional derivative step or sample clean-up. Biogenic amines were separated by the IonPac CS17 column, a cation-exchange column used with gradient elution, and detection was done by suppressed conductivity and mass spectrometry. Tyramine was simultaneously analysed by using a spectrophotometer (275 nm) before the suppressed conductivity detection. Linearity of response was obtained in the range 0.25-25 microg mL(-1). The detection limits ranged from 23 microg L(-1) for putrescine to 155 microg L(-1) for spermidine (suppressed conductivity) and from 9 microg L(-1) for agmatine to 34 microg L(-1) for spermidine (MS). Average recoveries from meat samples ranged from 85 to 97% and coefficients of variation ranged from 4.5 to 9.7%. The analysis of biogenic amines in fresh and processed meats (dry-cured, cooked and fermented products) can be used as a quality marker of raw material and for studying the relationship between their changes and the fermentation process involved in dry sausage ripening.     

复合式提取净化体系结合超高效液相色谱-串联质谱法检测畜禽肉中120种抗生素药物残留

建立了畜禽肉中兽药抗生素的复合式预处理方法，同时对8大类120种理化性质差异较大的目标化合物进行有效的提取和净化，并通过超高效液相色谱-串联质谱仪对其进行准确的筛查分析。样品经Na₂EDTA-Mcllvaine缓冲液溶解分散，由1.5%（v/v）甲酸乙腈提取，采用Oasis PRiME HLB通过式固相萃取、正己烷液液萃取两种方式先后对提取液进行净化。目标物在Atlantis^® T3色谱柱（100 mm×2.1 mm，3 μm）上，以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱分离，在正离子（ESI⁺）多反应监测（MRM）模式下进行定性定量分析。实验考察了不同pH条件的提取溶剂和不同净化方式对目标化合物回收率的影响并优化其条件。所建立的方法确保120种兽药在1.0~50.0 μg/L范围内线性关系良好，线性相关系数（r²）≥ 0.9953，其中89种化合物的r² ≥ 0.9990。7种化合物的定量限（LOQ）为10.0 μg/kg，21种化合物的LOQ为5.0 μg/kg，其余92种化合物的LOQ均≤ 2.0 μg/kg。低、中、高3个添加水平下的平均回收率为71.5%~109.2%，相对标准偏差为0.6%~15.3%。该方法灵敏高效，回收率优良，重复性稳定，适用于畜禽肉中多种抗生素药物的同时筛查检测。     

五灵脂及其炮制品的微量元素含量测定

为分析五灵脂生药及其炮制品中的微量元素，用电感耦合等离子体发射光谱法（ICP－AES）分析比较了五灵脂及其炮制品中15种微量元素的含量。结果表明，五灵脂生药及其炮制品中富含钙，镁，铁，炮制品可减少铝的溶出。     

基于QuEChERS提取的HPLC-MS/MS法测定禽肉中的利巴韦林与金刚烷胺

建立了液相色谱-串联质谱(HPLC-MS/MS)同时测定禽肉中利巴韦林和金刚烷胺的检测方法。禽肉样品用1%(体积分数)三氯乙酸水溶液-甲醇(1∶1,体积比)提取,经PCX固相萃取柱和QuEChERS方法净化后,以含5 mmol/L乙酸铵水溶液与甲醇为流动相梯度洗脱,BEH HILIC(2.1 mm×100 mm,1.7μm)色谱柱分离,电喷雾正离子模式电离,多级反应监测(MRM)模式进行检测,内标法定量。结果表明,利巴韦林和金刚烷胺在0.50~200μg/L范围内呈良好线性,相关系数均大于0.997。两种目标分析物的方法检出限(S/N≥3)分别为0.30μg/kg和0.15μg/kg,定量下限(S/N≥10)分别为1.00μg/kg和0.50μg/kg,样品在其1倍、2倍、10倍定量下限3个加标水平下的日内回收率为92.5%~104.7%,相对标准偏差(RSD)为3.4%~7.8%;日间回收率为93.3%~106.0%,RSD为6.0%~10.7%。该方法灵敏、简便、准确,可用于禽肉中利巴韦林和金刚烷胺残留的同时检测。     

在线固相萃取/高效液相色谱法检测熏烤鱼及熏烤肉制品中的多环芳烃

基于在线净化富集技术,建立了熏烤鱼和熏烤肉制品中15种欧盟优控多环芳烃的在线固相萃取/高效液相色谱-紫外/荧光(Online-SPE/HPLC-UV/FLD)检测方法。对提取溶剂和流动相进行优化,样品采用乙腈-丙酮(6∶4)匀浆处理,超声提取后,在线固相萃取柱Chrom Spher Pi(80 mm×3 mm)净化富集,反相C18PAH专用柱(250 mm×4.6 mm i.d.,5μm)分离,水、乙腈和异丙醇梯度洗脱,紫外和荧光检测器检测。结果表明,15种多环芳烃在相应的浓度范围内线性良好(r20.999);检出限为0.03~8.33μg/kg;熏烤鱼的回收率为67.4%~107.2%,相对标准偏差(RSD)为0.2%~7.7%;熏烤肉的回收率为71.8%~110.5%,RSD为0.8%~8.9%。经FAPAS质控样品验证,所测化合物种类和浓度范围均满足要求。