江苏沿海贝类软体中麻痹性贝毒素种类及含量变化的多年观测研究

Paralytic shellfish toxins(PSTs) are notorious neurotoxins that threaten public health and food safety worldwide.Although PST monitoring programs have recently been established throughout China, the profiles and variation of PSTs in important commercial clams(e.g., Mactra veneriformis, Ruditapes philippinarum, and Meretrix meretrix) along the Jiangsu Province coastline remain largely unexplored. In this study, a validated hydrophilic interaction liquid chromatography–tandem mass spectrometry(HILIC-MS/MS) method was used to examine PST profiles and levels in 540 clam samples from natural production areas along Jiangsu Province coastline during2014–2016. Although the PST levels(≤6.38 μg saxitotoxin equivalents(eq)/kg) were consistently below European Union regulatory limits(≤800 μg saxitotoxin eq/kg) during this time period, saxitotoxin, decarbamoylsaxitotoxin,and gonyautoxins 1 and 4 were detected, and nearly 40% of the samples were saxitotoxin-positive. The PST levels also varied significantly by seasons, with peak values observed in May during 2014–2016. This is the first systematic report of PSTs in clams from Jiangsu Province, and additional research and protective measures are needed to ensure the safety of clams harvested in this area.     

光合膜膜脂在八种海洋硅藻中的分布研究

利用超高效液相色谱-四级杆-飞行时间串联质谱(UPLC-Q-TOF-MS)对8种海洋硅藻的四种主要光合膜膜脂的分子结构和组成进行了定性定量分析。结果表明,海洋硅藻中MGDG含量最高,占四种光合膜膜脂的40%~70%左右,SQDG其次占10%~40%,而PG在4%~20%之间,DGDG占5%~20%;其中,各脂类分子的含量在0.14~99.79 nmol/mg干藻之间,而C_16:3/C_16:3-MGDG,C_20:5/C_16:3-MGDG,C_20:5/C_16:2-DGDG,C_20:5/C_16:1-DGDG,C_16:1/C_16:1-DGDG,C_14:0/C_14:0-SQDG,C_14:0/C_16:0-SQDG,C_14:0/16:1-SQDG,C_14:0/C_16:3-SQDG和C_18:1/C_18:1-PG等脂类分子在8种海洋硅藻的每一类膜脂中均有分布;与高等植物膜脂的脂肪酰基分布不同的是,海洋硅藻的MGDG与DGDG的sn-2位上的脂肪酸全部为C₁₆酸,可推断是通过类似高等植物典型的原核途径合成,而C₁₆酸和C₁₈酸在SQDG和PG的sn-2位上均有分布,可推断SQDG和PG存在原核和真核两种合成途径。     

蕾二歧灯芯柳珊瑚克生活性筛选及其低极性成分GC/MS分析

采用卤虫致死和细胞毒活性筛选模型,对蕾二歧灯芯柳珊瑚Dichotella gemmacea (valenciennes)乙醇提取物及各有机相进行了克生活性测定.结果表明,克生活性物质主要集中在石油醚相中.采用GC/MS技术对石油醚相进行了分析,鉴定了20个低极性化合物,主要为甾醇类、脂肪类化合物.推测甾醇类化合物是蕾二歧灯芯柳珊瑚的主要克生活性物质.     

2022年1月2日宁蒗MS 5.5地震现场新闻宣传启示

2022年1月2日云南省丽江市宁蒗县发生M_S 5.5地震。震后社会舆论关注度较高,相关话题一度冲上新浪微博热搜榜第十位。此时,因地震系统职责所在,运用新闻宣传手段快速、高效回复社会关切,既可还原地震事件真相、有效减少地震谣言的产生,亦能塑造地震行业的正面形象,从而更好地为防震减灾事业发展服务。     

2020年3月20日蒙古MS 5.9地震前地倾斜资料异常特征分析

采用形态法和小波分析法,分析2020年3月20日蒙古M_S 5.9地震震中距400 km范围内巴里坤、富蕴和芨芨台地震台倾斜观测资料的震前异常特征。结果表明：3套资料在震前均具有明显的中短期异常,分别表现为反向趋势变化、破年变形态和倾斜速率减缓的特征;使用db4小波对3套资料进行分析,其6—9阶在震前出现周期为几天至几十天的低频短期异常,同时巴里坤水平摆倾斜仪EW分量8—9阶趋势异常较显著。     

2022年6月1日芦山MS 6.1地震前地电阻率异常分析

利用归一化速率变化方法（NVRM）分析处理了芦山M_S 6.1地震震中距450 km范围内的成都地震基准台、冕宁地震台、红格地震台、甘孜地震台等4个台站的地电阻率观测数据,结果显示：红格地震台NS、EW测道及甘孜地震台NE测道原始数据震前出现年变趋势性下降,下降幅度为1%—3%;红格地震台NVRM曲线震前出现正异常,冕宁地震台、甘孜地震台出现负异常,曲线转折下降过程中发生芦山M_S 6.1地震。虽然整体而言提取出的地电阻率震前异常在时间上与此次地震对应关系较好,但甘孜地震台、红格地震台与此次地震震中间距离均大于300 km,提取出的异常是否为此次地震异常,还需进一步探究。     

土壤中痕量氨基甲酸酯和三唑类农药的样品提取方法研究

本文对比研究了QuEChERS、加速溶剂萃取和超声提取三种方法,结合液相色谱-串联质谱法解决了土壤中18种极性强、热稳定性差的痕量氨基甲酸酯和三唑类农药提取难题。研究表明,Qu ECh ERS法的基体加标回收率为76.3%~121.0%(除涕灭威为27.5%外),超声提取法为71.0%~100.0%(除涕灭威为4.7%,涕灭威亚砜为137.8%外),加速溶剂萃取法大多低于70%(甲硫威、涕灭威、三唑醇几乎没有回收),可见QuEChERS法比另两种提取方法结果更优,最终确定为检测氨基甲酸酯类和三唑类农药的样品提取方法。涕灭威回收率偏低、涕灭威亚砜回收率偏高与提取方法的热效应有关;仲丁威、甲萘威等组分的回收状况与土壤类型相关。     

Bias in the Determination of Zr,Y and Rare Earth Element Concentrations in Selected Silicate Rocks by ICP‐MS when Using Some Routine Acid Dissolution Procedures: Evidence from the GeoPT Proficiency Testing Programme

The analytical results for the modified river sediment, SdAR‐1 circulated in Round 31 of the GeoPT proficiency testing programme, revealed unexpected discrepancies for Zr, Y and most higher atomic number rare earth elements, in determinations made by ICP‐MS using acid attack digestion methods. This investigation compares these ICP‐MS results with those obtained for SdAR‐1 by three other methods: (a) ICP‐MS using fusion/sintering for sample digestion, (b) XRF analysis and (c) INAA. The distribution of results for the elements Rb, Sr, Ce, Y, Yb and Zr is examined and compared with those of the test material for Round 25 of GeoPT, Paraná basalt, HTB‐1. A substantial proportion (though not all) of Y, Yb and Zr determinations in SdAR‐1 by ICP‐MS/acid attack was variably low (sometimes very low) compared with other methods. A detailed evaluation of the procedures used to determine these results indicated that successful determinations by ICP‐MS/acid attack could be made if digestions were made at 180 °C for 48 hr using at least 2 ml HF per 100 mg of sample. We suggest that the more benign conditions (used by many laboratories) resulted in incomplete digestion of resistant minerals, such as zircon.     

A Rapid Method for Determining Boron Concentration (ID‐ICP‐MS) and δ11B (MC‐ICP‐MS) in Vegetation Samples after Microwave Digestion and Cation Exchange Chemical Purification

We present in this article a rapid method for B extraction, purification and accurate B concentration and δ¹¹B measurements by ID‐ICP‐MS and MC‐ICP‐MS, respectively, in different vegetation samples (bark, wood and tree leaves). We developed a rapid three‐step procedure including (1) microwave digestion, (2) cation exchange chromatography and (3) microsublimation. The entire procedure can be performed in a single working day and has shown to allow full B recovery yield and a measurement repeatability as low as 0.36‰ (± 2s) for isotope ratios. Uncertainties mostly originate from the cation exchange step but are independent of the nature of the vegetation sample. For δ¹¹B determination by MC‐ICP‐MS, the effect of chemical impurities in the loading sample solution has shown to be critical if the dissolved load exceeds 5 μg g^?1 of total salts or 25 μg g^?1 of DOC. Our results also demonstrate that the acid concentration in the sample loading solution can also induce critical isotopic bias by MC‐ICP‐MS if chemistry of the rinsing‐, bracketing calibrator‐ and sample solutions is not thoroughly adjusted. We applied this method to provide a series of δ¹¹B values of vegetal reference materials (NIST SRM 1570a = 25.74 ± 0.21‰; NIST 1547 = 40.12 ± 0.21‰; B2273 = 4.56 ± 0.15‰; BCR 060 = ?8.72 ± 0.16‰; NCS DC73349 = 16.43 ± 0.12‰).     

Combined Separation of Cu,Fe and Zn from Rock Matrices and Improved Analytical Protocols for Stable Isotope Determination

Isotope ratios of heavy elements vary on the 1/10000 level in high temperature materials, providing a fingerprint of the processes behind their origin. Ensuring that the measured isotope ratio is precise and accurate depends on employing an efficient chemical purification technique and optimised analytical protocols. Exploiting the disparate speciation of Cu, Fe and Zn in HCl and HNO₃, an anion exchange chromatography procedure using AG1‐×8 (200–400 mesh) and 0.4 × 7 cm Teflon columns was developed to separate them from each other and matrix elements in felsic rocks, basalts, peridotites and meteorites. It required only one pass through the resin to produce a quantitative and pure isolate, minimising preparation time, reagent consumption and total analytical blanks. A ThermoFinnigan Neptune Plus MC‐ICP‐MS with calibrator‐sample bracketing and an external element spike was used to correct for mass bias. Nickel was the external element in Cu and Fe measurements, while Cu corrected Zn isotopes. These corrections were made assuming that the mass bias for the spike and analyte element was identical, and it is shown that this did not introduce any artificial bias. Measurement reproducibilities were ± 0.03‰, ± 0.04‰ and ± 0.06‰ (2s) for δ⁵⁷Fe, δ⁶⁵Cu and δ⁶⁶Zn, respectively.