顶空气相色谱-质谱法测定布南色林原料药中遗传毒性杂质

目的：建立顶空气相色谱-质谱法测定布南色林原料药中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯3种遗传毒性杂质含量的方法。方法：采用顶空气相色谱-质谱法，以甲磺酸丁酯为内标，按内标标准曲线法进行甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯的含量测定。色谱条件：DB-WAX毛细管色谱柱（30 m×0.25 mm×0.25 μm）；程序升温，初始柱温为40℃，维持3 min，升温速率为30℃·min^-1，终止温度150℃，保持2 min；进样口温度为110℃；载气（He）流速为0.6 mL·min^-1；进样量为1 mL；进样方式为分流进样，分流比为20：1。质谱条件：电子轰击离子源（EI），扫描方式为选择性离子检测；离子源温度为200℃；接口温度为150℃；电子能量为70 eV；溶剂延迟1 min。结果：3种杂质成分之间的分离度均大于2.0；甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯检测质量浓度线性范围均为0.025~3.0 μg·mL^-1（r ≥ 0.998 5）；精密度、稳定性、重复性试验的RSD<5%；加样回收率分别为93.40%~101.40%（RSD为3.2%，n=9）、92.80%~99.70%（RSD为2.5%，n=9）和96.30%~100.75%（RSD为1.6%，n=9）。结论：该方法简便、准确、灵敏、迅速，可用于布南色林原料药中3种遗传毒性杂质的测定。     

Determination of polycyclic aromatic hydrocarbons (PAHs) in cosmetic products by gas chromatography-tandem mass spectrometry

A gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) method is developed to determine 18 representative polycyclic aromatic hydrocarbons (PAHs) in cosmetics, including Benzo[a]pyrene (BaP) and others. The method offers high sensitivity and selectivity under selected reaction monitoring (SRM) mode to satisfy the requirements of both quantitation and qualitation. The extraction solvent system used in this study is acetone/hexane 1:1 (v/v) and other purification procedure is unnecessary. The linearities of 18 PAHs are validated in different concentration in the range of 0.25–20 ng/mL individually with coefficient correlation (r) higher than 0.996. The recoveries for spiking 3 different concentrations are from 87.40% to 120.44% for 18 PAHs and the coefficient of variation (CV) are below 12.32%. Limit of quantification (LOQ) of 18 PAHs is in the range of 0.05–0.2 mg/kg. A matrix enhancement effect is observed and can be compensated with deuterated internal standard. The method has been successfully applied to 73 samples, over 40 of them are lipsticks. The results show none of the samples detect Benzo[a]pyrene (BaP) and Dibenzo[a,h]anthracene (DBA), both are classified as the most carcinogenic. 8 PAHs are detected and the average value between 0.08 and 0.27 mg/kg. This study offers a sensitive and simple method to analyze 18 representative PAHs successfully and can be applied to cosmetic products and raw materials.     

An experimentally supported, mathematical explanation of the gas chromatographic elution behaviour of the long-chain carbon members of the homologous series

By substituting the saturated vapour phase tension of the pure normal hydrocarbons described by the Clausius-Clapeyron law into the accepted expression of the specific retention volume (V_g,T), a theoretically coherent and relatively simple mathematical evidence of the elution behaviour of the homologous members has been deduced. It gives exponential retention time dependence on carbon number for isothermal, and nearly equidistant (i.e., approximately linear retention-time dependence on carbon number) elution for linear temperature programmed gas chromatographic runs. The final equations are in close correlation with the experimental results. Special emphasis is placed on the fact that a good approximation—not strict physical laws—have been found.     

天然冰片在小鼠组织内的GC—MS测定法和组织分布研究

目的：建立天然冰片在小鼠组织内含量测定的GC—MS法并进行组织分布研究，初步探索天然冰片的归经特征。方法：采用DB-5MS弹性毛细管色谱柱（0．25mm×30m×0．25μm）；电子轰击（E1）电离方式，轰击能量为70eV，倍增电压1100V；选择性离子检测（SIM），天然冰片m／z95，内标萘m／z128；小鼠组织样品用生理盐水匀浆后，加入萘作为内标，用正己烷振荡萃取，取上清液进样测定。组织分布研究以天然冰片的CMC—Na溶液给小鼠灌胃，在不同时间点分批处死小鼠后取各组织样本，经处理后用GC—MS法测定组织中的天然冰片含量。结果：本研究建立的天然冰片GC—MS测定方法，在22ng·mL^-1 -22μg·mL^-1范围内响应信号（Y）与天然冰片浓度（X）呈良好线性关系，Y=0．000486X＋0．00036，R^2=0．999（n=3），最低检测限为10ng·mL^-1，定量下限为22ng·mL^-1，日内精密度为3．72—6．11％，日间精密度为7．29～17．6％，相对回收率和提取回收率分别为85．95～107．93％和93．04～103．03％。组织分布研究结果表明，天然冰片分布于大部分组织，单个组织内天然冰片浓度随时间延长呈现多峰现象；天然冰片在肝脏内含量最高，在心、脑、肾等重要组织内的含量也较高。结论：本研究建立的GC—MS测定方法准确、可靠，可用于天然冰片在动物体内的定量分析；天然冰片在不同组织内的分布有明显差异，肝、肾、心、脑中分布含量较高；天然冰片的归经特征中有归心经的趋势。     

鸢尾中鸢尾酮的鉴定及含量测定

目的 建立鸢尾中鸢尾酮的鉴定和分析方法。方法 采用气相色谱-质谱法鉴定了鸢尾酮的3种异构体，并采用气相色谱法测定了鸢尾浸膏中鸢尾酮的含量。结果 根据质谱裂解规律鉴定了3种鸢尾酮的异构体：α-、β-、γ-鸢尾酮，并且鸢尾浸膏中主要含γ-鸢尾酮。两批鸢尾中鸢尾酮的质量分数分别为687、238μg/g(n=6)，质量分数差异较大。结论 采用气相色谱一质谱法和气相色谱法分析鸢尾中鸢尾酮，方法高效、准确，分析时间适中。     

雷公藤和昆明山海棠植物中挥发性化学成分比较

雷公藤(Tripterygium wilfordii Hook.f.)为卫矛科雷公藤属植物的一种,分布在我国长江以南诸省区。民间早期用其治疗类风湿性关节炎,现已用于多系统疾病的治疗。雷公藤的主要成分包括二萜类、三萜类、倍半萜类和生物碱。近年来,雷公藤的多种药理作用引起广大科研人员的关注,同时,也促进了同属     

栝楼子挥发油的成分分析及其生物活性的初步研究

目的:分析栝楼子挥发油成分并检测其生物活性。方法:采用水蒸汽蒸馏法提取,气相色谱-质谱联用法进行成分分析,并分别用测A值和MTT法检测其抑菌和细胞毒生物活性。结果∶从分离的挥发油化合物中,鉴定出42个化合物,占挥发油总相对含量的79.434%。挥发油对金黄色葡萄球菌、大肠杆菌有较好的抑制作用;对真菌红酵母有显著的抑制作用,在800μg·mL^-1时抑制率达到90.91%;对肿瘤胃癌细胞株SGC-7901细胞也有显著的细胞毒活性,浓度为50μg·mL^-1时,抑制率高达86.13%。结论:首次从挥发油的角度来研究栝楼的药理作用,其挥发油有抑菌活性和对胃癌细胞株SGC-7901细胞有很好的细胞毒活性。     

桃仁脂肪酸GC-MS指纹图谱研究

目的：对桃仁脂肪酸进行气相色谱指纹图谱研究，为桃仁的质量评价提供依据。方法：利用毛细管气相色谱对桃仁脂肪酸进行分析,并利用GC-MS 技术确认指纹图谱中的特征指纹信息，进行系统聚类和相似度分析。结果：对34批不同产地、品种的桃仁进行了测定，获得了较为理想的包含特征信息的桃仁GC 指纹图谱。结论：本方法重复性好，所建立的指纹图谱为桃仁药材的质量控制提供了有效手段。     

气相色谱-串联质谱法测定血清中的16种多环芳烃

目的 建立血清中16种多环芳烃的气相色谱-串联质谱测定方法。方法 血清样经甲醇沉淀蛋白,加入正己烷与二氯甲烷混合溶剂萃取,萃取物氮吹至近干后,正己烷和二氯甲烷混合溶剂复溶,取1 μl上清液进样分析。16种待测多环芳烃经DB-5色谱柱(30 m×0.25 mm,0.25 μm)分离,多反应监测模式监测,内标法定量。结果 本法在1.0 μg/L～2.0×10² μg/L范围内线性良好,方法检出限为4.20×10^-2 μg/L～0.27 μg/L,加标回收率为79.7%～108.0%,精密度为2.57%～6.76%。结论 本方法具有灵敏、快速、回收率和重复性好等优点,满足人血清中多种多环芳烃测定的要求。     

Analysis of Serum Fatty Acids Profile in Kidney Transplant Recipients

Patients with end-stage kidney disease, treated with renal transplantation, are at increased risk of cardio-vascular disease (CVD) and cardio-vascular mortality. They are also characterized by an atherogenic dyslipidemia. Alterations of the fatty acids (FA) profile contribute to increased cardio-vascular risk in the general population. In the current study we test the hypothesis that kidney transplantation is associated with ab-normalities in FA profile. FA profile was analysed by gas chromatography–mass spectrometry in 198 renal transplant recipients, and 48 control subjects. The most profound differences between renal transplant patients and controls were related to the content of branched chain FA, monounsaturated FA, and n-6 polyunsaturated FA, respectively. The FA profile significantly separated the patients from the controls in the principal component analysis (PCA). The abnormalities of FA profile showed a tendency for normalization in long-term kidney recipients, as compared to patients with recent transplants. The n-3 PUFA content demonstrated a strong inverse association with the presence of inflammation. Most profound alterations of the FA profile were observed in patients with impaired graft function (glomerular filtration rate < 45 mL/min). The study demonstrated significant disorders of the FA profile in kidney transplant recipients, that might contribute to cardio-vascular risk in this vulnerable patient population.