OBJECTIVE:To establishe an analysis and identification method for 2-methylisoborneol(2-MIB) and geosmin(GSM) in water using purge and trap-gas chromatography-mass spectrometry.METHODS:The samples were enriched and analyzed using a purge and trap system, followed by the separation on a DB-624(30 m×0.25 mm, 1.4 μm) chromatographic column. Quantification was performed using gas chromatography-mass spectrometry with the selected ion monitoring and internal standard calibration.RESULTS:The calibration curves for 2-MIB and GSM showed an excellent linearity in the range of 1 to 100 ng/L with R~2 values greater than 0.999. The detection limit and quantification limit for both 2-MIB and GSM were 0.33 ng/L and 1.0 ng/L, respectively. Spike recovery experiments were further carried on the source water and drinking water at three concentration levels. It showed that the average recoveries were from 82.0% to 111.0% for 2-MIB while 84.0% to 110% for GSM. Additionally, the test precision of 2-MIB and GSM ranged from 1.9% to 7.3% and 1.9% to 5.0%(n=6), respectively. The analysis of multiple samples including the local source water, treated water and distribution network water confirmed the existence of 2-MIB and GSM.CONCLUSION:Compared to the national standard(GB/T 5750.8-2023), the proposed method enables fully automated sample introduction and analysis without the extra pre-treatment. It provides the advantages of simplicity, good repeatability and high accuracy.

OBJECTIVE:To develop a method which is used for rapid determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) and 16 kinds of phthalates(PAEs) in tap water by stirring rod adsorption extraction(SBSE) combined with gas chromatography-mass spectrometry(GC-MS). METHODS:The twister mixing rod coated with polydimethylsiloxane(PDMS) and ethylene glycol-polydimethylsiloxane(EG-silicone) was used to enrich analyte from 50 mL tap water. The twister mixing rod coated with EG-silicone was directly placed into the sample bottle containing 50 mL of tap water, while fixing the PDMS stir bar on the inner wall of the sample bottle and immersing it in the liquid. Add 5%(W/V) sodium chloride to the sample bottle, followed by adding 5% methanol. Stir at room temperature for 2 hours for extraction. Next, remove the mixing stick and dry its surface. The pre-prepared SBSE was analyzed by TD-GC/MS, with the optimized thermal desorption conditions: desorption temperature 275 ℃, desorption time 15 min, cryofocusing temperature-40 ℃. RESULTS:Regression equations revealed acceptable linearity(correlation coefficients >0.986) across the working-standard range from 200-2000 ng/L for the 32 analytes. The limits of detection(LODs)were further evaluated were from 1.13-121 ng/L. With the optimized pretreatment method, the spiked recoveries of tap samples(200 and 2000 ng/L)were in the range of 62.5%-98.4% with the relative standard deviations(RSDs) of 3.5%-25.3%. CONCLUSION:The established method can realize the rapid detection of high throughput in the laboratory, it is simple, convenient to operate, and the extraction and analysis time is short.

A method for the determination of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in smoked meat samples by saponification/solid-phase extraction and gas chromatography-mass spectrometry has been developed. Both saponification and solid-phase extraction conditions were optimized, which lead to shorter sample preparation time and excellent sensitivity and selectivity. The optimal saponification condition for the lipid extract of 5.00 g smoked food sample was 5 mL KOH (1.5 mol/L)-ethanol at 70°C for 5 min, and the shorter alkaline treatment time avoided the loss of volatile EUPAHs such as Benzo[c]fluorene. All the EUPAHs showed good linearity in the range between 5.0 and 50.0 ng/mL with correlation coefficients between 0.997 and 1.00. The estimated LODs for the EUPAHs were 0.15-0.30 μg/kg, while the LOQs were 0.50-1.0 μg/kg. The three spiking levels of EUPAHs were 1.0, 2.0 and 5.0 μg/kg, and the average recovery was between 75.2 and 99.6%, while the RSD were 2.3-12.4%. This sensitive and rapid method was successfully applied to smoked meat samples from Zhejiang Province of China, and the results revealed the presence of 13 EUPAHs. Benzo[a]pyrene (BaP) was found in 19 out of 20 samples, with concentration ranging from 0.51 to 4.57 μg/kg. The sum of concentrations of PAH4 (summation of benzo(a)pyrene, chrysene, benzo(a)anthracene, and benzo(b)fluoranthene) were 2.40-53.56 μg/kg.

目的 比较过氧化氢-乙醇消毒液对噬菌体和脊髓灰质炎病毒的灭活效果,初步评估噬菌体代替脊髓灰质炎病毒评价消毒剂对病毒灭活效果的可行性.方法 采用试管内悬液法,观察过氧化氢-乙醇消毒液对大肠埃希菌噬菌体(ΦX174)和脊髓灰质炎病毒(疫苗株PV-I)的消毒效果.结果 在非清洁模式下(有机干扰物为30 g/L牛血清白蛋白),该消毒液作用1.0 min,对悬液中大肠埃希菌噬菌体和脊髓灰质炎病毒的灭活对数值均＞4.00.结论 过氧化氢-乙醇消毒液对噬菌体和脊髓灰质炎病毒灭活效果一致,检测方法更为快捷、方便,对试验设备、人员的要求相对较低,初步推论可用于消毒液病毒灭活效果的观察.

目的 利用全自动流动注射分光光度法(异烟酸-巴比妥酸法)和顶空-气相色谱法分别测定水中总氰化物,并对2种方法进行分析比较.方法 流动注射法中,样品液在酸性介质中经高温紫外消解,氰化物以氰化氢的形式蒸馏出来后,被碱性溶液吸收,在弱酸性条件下与氯胺-T反应生成氯化氰,再与异烟酸反应,经水解生成的戊烯二醛与巴比妥酸缩合成蓝紫色燃料,600 nm处比色检测;顶空-气相色谱法中,酸性条件下,氯胺-T与水中总氰化物发生衍生反应生成氯化氰,顶空进样,气相色谱电子捕获检测器检测,外标法定量.结果 全自动流动注射法和顶空-气相色谱法,在一定浓度范围内,总氰化物浓度与峰面积的线性关系良好;流动注射法中,当添加浓度在4.0 μg/L～20.0μg/L时,加标回收率为91.9％～93.9％,标准变异系数(RSD)＜2.31％;顶空-气相色谱法中,在0.5 μg/L～10.0 μg/L的标准添加浓度内,加标回收率最低为89.5％,最高为94.9％.结论 2种方法测定水中总氰化物的灵敏度、精密度、准确度均符合国家《生活饮用水卫生标准》的检测要求.流动注射法适合大批量样品检测,分析速度更快,但试剂配制繁琐,费液产生较多.顶空-气相色谱法的检测灵敏度更高,所用试剂少,操作简单,环境污染小.

This work aimed to establish a novel determination method for acrylamide in coffee and its products by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Acrylamide in samples were prepared by a single-step solid-phase extraction clean-up using mixed mode sorbents. The bromine derivatization efficiency of acrylamide and its internal standard were improved at an acidic condition. After derivation, the retention capability of acrylamide and its resistance to interference were significantly improved. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.2 and 4 μg/kg for roasted and instant coffees, while they were 0.24 and 0.8 μg/kg for ready-to-drink coffees. The average recoveries for acrylamide ranged from 99.3 to 102.2% in coffee and its products. All the results showed that the developed method was simple, quick, specific and suitable for screening and determination of acrylamide in batch samples of coffee and its products.

目的建立气相色谱质谱联用法同时测定水中2, 4, 6-三氯酚、五氯酚、2, 4-二氯苯氧乙酸（2, 4-D）和灭草松。方法水样过HLB固相萃取柱富集,以10 m L/min速度上样,二氯甲烷洗脱,氮吹浓缩后,用0.1 g/L抗坏血酸甲醇溶液100μL和0.2 mol/L三甲基氢氧化硫甲醇溶液10μL 40℃衍生40 min,用气相色谱-质谱联用法分离和检测,内标法定量。结果方法在0.05～0.50 mg/L范围内线性关系良好,相关系数均大于0.999 0,检出限为2～3 ng/L,定量限为8～12 ng/L,回收率为74.8%～99.6%,相对标准偏差为0.9%～6.7%（n=6）。结论本方法适用于水中2, 4, 6-三氯酚、五氯酚、2, 4-D和灭草松的快速测定。

目的 建立全自动固相萃取-气质联用法同时检测水体中16种多环芳烃的分析方法.方法 首先对萃取柱种类、萃取方法、水样初始pH值和体积等条件进行优化.水样经磷酸调节pH值至2,抗坏血酸消除余氯干扰,MIP-PAHs固相萃取柱富集、净化,甲醇淋洗,二氯甲烷洗脱,通过气相色谱-质谱联用仪对样品中的16种多环芳烃进行检测分析.结果 气相色谱-质谱联用法对自来水中16种多环芳烃的检测效果较好,回收率在82.8％ ～ 109.3％.在5 μg/L～ 250 μg/L质量浓度范围内,多环芳烃的峰面积与对应质量浓度呈良好线性关系,相关系数(r2)均在0.999以上,检出限均不大于0.37 μg/L,相对标准偏差(RSD,n=5)为1.0％ ～6.8％.结论 所建立气相色谱-质谱联用法对自来水中16中多环芳烃的检测方法自动化程度高,快速、灵敏、简单,适用于快速分析环境水样中的痕量多环芳烃.

OBJECTIVE:A gas chromatography-mass spectrometry(GC-MS) method for the determination of 16 European priority polycyclic aromatic hydrocarbons(16 EUPAHs) in infant formula milk powder was established, and the characterization and investigation of 16 EUPAHs in 70 milk formula powders were carried out in 2020.METHODS:After hydrolysis, extraction, saponification and solid phase extraction, infant formula milk powder was detected by GC-MS using DB-EUPAH capillary column(20 m×0.18 mm, 0.14 μm)and quantified by internal standard method.RESULTS:The average recoveries ranged from 67.8% to 116.2% and the relative standard deviations ranged from 2.0% to 15.1%(n=6). The limits of quantification and detection of the method were 0.5 and 0.2 μg/kg, respectively. The content of 16 EUPAHs was <0.2-0.48 μg/kg, including PAH4 content in the range of <0.2-0.91 μg/kg, the characterization and investigation of infant formula powder in 16 EUPAHs mainly chrysene, cyclopenta[c, d]pyrene, benz[a]anthracene, benzo[b]fluoranthene, benzo[g, h, i]perylene.CONCLUSION:The method is simple, accurate and suitable for the determination of 16 EUPAHs in infant formula milk powder. The result showed that the content of 16 EUPAHs in commercially available infant formula milk powder in Hangzhou was low and all of them met the limit requirement of European Union.

目的 建立全自动固相萃取-气相色谱-质谱法检测水中6种苯氧羧酸类除草剂的方法.方法 取水样1L,加抗坏血酸除余氯,经浓盐酸调节pH＜1.0,加D3-2,4 二氯苯氧乙酸(D3-2,4-D)内标后混匀,经全自动固相萃取仪上HLB 固相萃取柱萃取,用二氯甲烷洗脱固相萃取柱上吸附的待测物,洗脱液氮吹至1 ml,用三甲基氢氧化硫溶液衍生,GC-MS分离检测.结果 水样中的苯氧羧酸类除草剂的浓度在10 μg/L～100 μg/L线性良好,方法检出限为0.003 μg/L,平均加标回收率为90.0％～103.1％,相对标准偏差(RSD)为3.15％～5.82％.结论 该方法简便、准确,适用于水中6 种苯氧羧酸类除草剂的检测.

目的 优化水源水中2种微囊藻毒素(MC-LR和MC-RR)的双柱净化-高效液相色谱分析方法,去除水源水中的干扰物质,减少原有方法检出的假阳性及假阴性的概率并用于水样的实际测定.方法 样品滤液和乙酸提取藻细胞液体合并后,经HLB固相萃取柱富集洗脱,经氮吹至近干后,用甲醇定容至1.0ml,定容液经SLH固相萃取柱净化,经甲醇淋洗,甲醇(含0.1％三氟乙酸)洗脱,洗脱液吹至近干,流动相定容至1.0ml,进样分析.结果 MC-LR和MC-RR的线性范围为0.30 μg/L～5.00μg/L,线性相关系数≥0.9997,检出限为0.10 μg,/L～0.13 μg/L,加标浓度为0.30 μg/L～5.00 μg/L时,平均回收率为83.39％～108.1％;相对标准偏差(RSD)为1.45％～8.69％(n=6).结论 该法对检测用仪器要求不高、干扰少、准确率高,适用于基层单位对水源水等杂质较多水样中微囊藻毒素的检测.

The purpose of this research was to determine the occurrence of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in various types of tea purchased on Hangzhou city market in China in order to control their safety. The results indicated that the incidence rate of EUPAHs compounds was 97.4%. The total EUPAHs levels ranged from 1.2 mu g/kg to 155.6 mu g/kg, with a median of 27.1 mu g/kg and a mean of 42.3 mu g/kg. Cyclopental[cd]pyrene was not only the most frequently detected EUPAH but also detected at the highest concentrations with a mean of 12.2 mu g/kg. The 4-membered and 5-membered ring EUPAHs were detected in nearly all of the tea types and accounted for 83.4% to 100.0% of the total EUPAHs mass distribution. The transfer percentages of EUPAHs from the various tea leaves to tea infusions and effect of infusion time were investigated as well. A transfer rate between 5.9% and 24.2% was found for the EUPAHs and these levels were within the maximum safe consumption limits for drinking water according to European Union regulations (EU Council Directive 98/83/EC).

Objective To study the disinfection effect of Ortho-phthalaldehyde( OPA) on bacteria spores and mycobacterium,and to evaluate the stability of the OPA during continuous use. Methods The germicidal effect of OPA on Bacillus subtilis var. niger spores and Mycobacterium chelonei subsp. abscessus were evaluated by suspension quantitative bactericidal test. Results When using 4 800 mg/L OPA to treat B. subtitle var. niger spores for fourteen hours and M. chelonei subsp.abscessus for 5 mins,the killing log value was 7. 65 and 4. 60 respectively. When using 3 000 mg/L OPA to treat B. subtitle var. niger spores for 14 hours and M. chelonei subsp. abscessus for 5 mins,the killing log value was 4. 02 and 2. 88 respectively. The germicidal effect of OPA was stable when continuously being used for immersion of instruments for 14 days. While the germicidal effect could not reach high level disinfection effect when continuously being used in endoscopic cleaning machine for 14 days,with the total number of treated endoscope of 80 strips. Conclusion The working concentration offered by manufacturer is not appropriate for high level disinfection of medical instrument.

目的 比较测定冻干血铬电感耦合等离子体质谱法(ICP-MS)和石墨炉原子吸收法(GFAAS),为血中铬的测定提供参考.方法 将冻干粉用2.0 mL的纯水溶液复溶后,吸取一定体积的样品用0.2％TritonX-100和1％硝酸溶液直接稀释25倍后,应用ICP-MS和GFAAS测定铬含量并比较.结果 ICP-MS和GFASS分别在0～10.0 μg/L和0～3.0 μg/L的线性范围内的相关系数均＞ 0.999,ICP-MS检出限为0.15 μg/L,GFASS为0.35 μg/L;2种方法的精密度和准确度均符合要求,ICP-MS相对标准偏差＜5％,GFAAS的相对标准偏差在5％左右,对定值冻干血铬的测定,结果均在定值范围内;选取高、低浓度的各12份冻干血铬进行测试,2种方法检测结果比较差异无统计学意义(P＞0.05).结论 ICP-MS和GFAAS均可满足冻干粉中血铬的检测要求,但ICP-MS可同时进行多元素分析,也可快速测定血液生物样品,更适用于血中铬元素的测定.

目的 优化《化妆品安全技术规范》中的苯基苯并咪唑磺酸等15种组分的检测方法,使其可以准确测定出实际样品中T150、T-M和T-S3种防晒剂成分的含量.方法 采用四氢呋喃提取化妆品并过滤,AQ-C18色谱柱(4.6 mm×250 mm,5μm)分离.以甲醇、四氢呋喃-高氯酸(300∶0.2,V/V)为色谱分离流动相进行梯度洗脱,经二极管阵列检测器检测.结果 15种防晒剂均能准确定量,各组分在1.274 μg/ml ～1 033.2μg/ml呈良好线性关系,相关系数(r) ≥0.999 6,回收率为93.8％～ 114.0％,相对标准偏差(RSD)为1.64％～4.59％.结论 本法能对实际样品中的T150、T-M和T-S3种防晒剂成分准确定量,有助于更好地监督特殊类化妆品的质量.

Objective To establish a method for the rapid and simultaneous determination of 16 metal elements in whole blood by inductively coupled plasma-mass spectrometry (ICP-MS).Methods After the whole blood samples were diluted in a mixed solution containing 1％ nitric acid and 0.1％ Triton X-100,16 trace metal elements in whole blood samples including Pb,Cd,Be,Ba,Mn,Cu,Zn,Mo,Co,Ni,Se,As,Sb,V,Ag,Cr were simultaneously determined by ICP-MS with hexapole collision cell technology,with 209Bi and 89y as the internal standard elements.The whole blood trace element standard substance was used for the quality control.Results All of the average correlation coefficients (r) were greater than 0.999 0,indicating a good linearity.The detection limit of the 16 elements was within 0.002 μg/L-0.70 μg/L.The recovery rates of each element varied from 89.2％ to 113.5％.The inter-day and intra-day precision was within 3.23％-10.96％ and 0.46％-9.29％,respectively.Conclusion The method is simple and rapid,and provided the accurate and satisfied results.It meets the technical requirements of biology samples and can be applied to the determination of 16 metal elements in whole blood samples.

目的 建立消毒产品中30种糖皮质激素的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法.方法 以饱和氯化钠溶液及乙腈2次液液萃取样品后做沉淀蛋白处理,提取液经过固相萃取小柱净化浓度后采用C18色谱柱分离(100 mm×2.1 mm,1.7 μm).以乙腈和水(含0.1％甲酸)为色谱分离流动相进行梯度洗脱,多反应监测模式进行定性分析和定量分析.结果 30种糖皮质激素以标准曲线-外标法定量,其在0 ng/ml～50.0 ng/ml时,线性关系良好,相关系数(r) ≥0.995;定量限(S/N=10)为0.002 ng/ml～0.6 ng/ml.分别加入浓度为5.0 ng/ml和25.0 ng/ml的标准溶液,其回收率为58.7％ ～ 146.8％,相对标准偏差(RSD)为1.22％ ～ 19.21％.结论 本法操作简便、灵敏度高,适用于消毒产品中糖皮质激素的检测.

目的 建立大气PM2.5中3种硝基多环芳烃的气相色谱-串联二级质谱测定法.方法 大气PM2.5经石英滤纸采集,待测化合物用二氯甲烷-丙酮有机溶剂提取,提取液用旋转蒸发仪浓缩至1.0 ml;经中性硅胶柱净化,收集洗脱液浓缩至1.0 ml,用气相色谱-串联二级质谱法检测.结果 2-硝基荧蒽的检出限为2 ng/ml,3-硝基荧蒽、1-硝基芘的检出限为5 ng/ml;2-硝基荧蒽的最低检出浓度为1 pg/m3,3-硝基荧蒽、1-硝基芘的最低检出浓度为3 pg/m3(采样体积以1 500 m3计).3种硝基多环芳烃的加标回收率为88.5％ ～ 96.0％,相对标准偏差(RSD)为2.0％～5.2％.结论 该方法操作简便、灵敏度高,适用于PM2.5中3种硝基多环芳烃的测定.

目的建立全自动固相萃取-气相色谱法检测水中2,4-滴的方法。方法取1 L水样,加浓硫酸使水样p H＜1,通过全自动固相萃取仪以15 ml/min将水样过HLB固相萃取柱（Waters,500 mg,Oasis）萃取,用0.1 mol/L Na OH甲醇溶液洗脱HLB固相萃取柱上吸附的待测物,氮气吹干,用三氟化硼甲醇溶液衍生后,加纯水用正己烷提取,经气相色谱仪进行检测。结果水样中2,4-滴的浓度为0μg/ml~1.0μg/ml时,与峰面积呈良好的线性关系,相关系数（r）均＞0.999,最低检出浓度为0.01μg/L（1 L水样）。0.1μg/L加标水样组2,4-滴的回收率为110.0%,相对标准偏差（RSD）为6.9%;1.0μg/L加标水样组2,4-滴的回收率为106.0%,RSD为2.3%。结论该方法简便、准确,适用于水中2,4-滴的检测。