工作场所空气中氨基磺酸铵的离子谱测定法

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工作场所空气中氨基磺酸铵的离子谱测定法
关维俊白玉萍徐国卉庞淑兰陈刚
·监测与检验技术·
【摘要】目的建立T作场所空气中氨基磺酸铵的检测方法。方法样品用混合纤维滤膜采集,
用水洗脱,离子谱检测磺酸根离子。通过测试疗法的线性范围、检}l{限、精密度、准确度、洗脱效率和
样品稳定性来评价该方法的可行性。结果该厅法的线性范嗣0.Ol~0.2mg/ml,相关系数r--0.9998;检
I叶{限2.25Ixs/ml,最低检出浓度为0.75mg/m1;半均相对标准偏差3.95%,平均回收率99.1%。洗脱效
率98.2%。结论该标准方法操作简便,精密度、回收率、洗脱效率及样品稳定性能够满足“工作场所
空气中有毒物质检测方法的研制规范”要求,能准确测定工作场所空气中氨基磺酸铵的含量。
【关键词】磺酸类;谱法,离子交换;工作场所
氨基磺酸铵可用作非选择性除草剂、电镀液、合成N20等。在生产环境中主要以细小颗粒状悬浮在窄气中。动物实验证实,氨基磺酸铵属于低毒物质,我闰已将其列入工作场所有害凶素职业接触限值的同家U生标准,时间加权容许浓度(PC.TWA)为6mg/m3,短时接触容许浓度(PC.STEL)为15mg/m,。目前,采集生产环境空气中氨基磺酸铵丰要用低流量空气收集器,混合纤维滤膜或微孑L滤膜进行采集。检测方法主要有亚硝酸钠比法定馈氨基磺酸、Nessler’s法定量氨离子、离子潜法检测氨基磺酸根,美国劳工部职业安全卫生管理局颁布的标准方法为离子谱法检测氨基磺酸根。根据我1日丁作场所有毒有害物质检测方法的研制规范要求,我们参照该方法提供的分析条件,使用离子谱仪对该方法的检ff{限、线性关系及范嗣、精密度和准确度、样品稳定性等方匝i进行研究。
一、材料与方法
空气中氨基磺酸铵用混合纤维滤膜或微孔滤膜进行采集,用水洗脱后,经阴离子谱柱分离,用离子谱检测定量。
1.仪器:DIONEX犁离子谱仪(美国戴安公司),AKFC.92A型粉尘采样器、KQ.250型超声波清洗器、微量移液器、混合纤维滤膜(直径37mm、孔径0.8mm),孑L径0.45p,m的一次性滤器等。
2.试剂:氨基磺酸铵标准对照品(纯度99%)由中国疾病控制中心提供。试验用水为纯水器制纯水。
3.采样:(1)长时间采样(实验室模拟):将采样夹安装在采样器上,采样器垂直放在1.5m高度,避免阳光直射。以2.0L/min的流量连续采集8h(960L)。注意观察流量变化。(2)短时问采样:采样方法同长时间采样,以5.0L/min的流量采集15rain(75L)。采样结束后将滤膜折叠(采样面朝罩),用干净的镊子夹取滤膜放入具寒比管中。带回实验窒分析。(3)个体采样:连接个体空气收集器与采样头,将采样
DO!:10.3760h‘maj.issn.1001—9391.2010.02.020
作者单位:063000唐IJI,华北煤炭医学院预防医学系头夹在工人的农领上,采样器垂直放在丁人的呼吸带高度,避免阳光直射。以2.0L/min的流速连续采集8h(960L)。注意观察流量变化。
4.分析步骤:(1)样品前处理:取采样后的滤膜置于25IIIl干净的具塞玻璃试管中,加去离子水定容至25ml,盖紧管塞。置超声清洗器中超声振荡20min。用注射器吸取洗脱液通过0.45斗m的滤膜,除去样品中的颗粒物质。(2)标准曲线的绘制:氨基磺酸铵标准溶液的配制:准确称取氨基磺酸铵标准品650mg。加水定容至25IIll,浓度为650ms/25ml(26mg/m1)。分别吸取标准储备液(26mg/m1)25、50、75、100、125、150斗I,分别加水定容至25IIll,其浓度分别为650、1300、1950、2600、3250、3900斗S/25ml。分析条件:谱柱:ASRS250mmx4mm阴离子柱;EG40淋洗液发生器(氢氧化钾),H:O=20:l;流速:1.0ml/min;EDSO电化学检测器;自动进样,进样量25“l。保留时间为3.5min。取上述标准系列3IIIl左右置于自动进样瓶内,重复进样3次,以保留时间定性,以3次测定值的峰面积均值与对应的氨基磺酸铵的浓度计算回归方程与相关系数。回归方程为P=0.025X-0.1031,相关系数为0.9998。
5.样品测定:将采样后的滤膜置于25IIIl具塞比管中,加入纯水定容至25rIll,置超声清洗器中,振荡20min。取洗脱液按标准曲线绘制方法进行操作。将峰面积代入回归方程(或查标准曲线)得样品中氨基磺酸铵的浓度。
6.计算:按下式将采样体积换算成标准采样体积:Vo=V。器×击
式中:V广标准采样体积(L);V。——在温度为t(℃),大气压为P时的采样体积(L);£——采样点温度(℃);P——采样点的大气压力(kPa)。
按下式计算空气中氨基磺酸铵的浓度:
C2
yc。
式中:C一夺气中氨基磺酸铵的浓度(ms/m,);c一测得洗脱液中氨基磺酸铵的浓度(tLs/m1);y旷一标准采样体积(L)。
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由标准曲线浓度与峰高的对应值求出分析物的浓度,用
斗g/25
ml表示。不需要进行体积换算,因为被分析物与标准樱桃采摘机
溶液的体积是一致的。
二、结果与讨论
1.谱条件的选择:原方法使用的仪器配有电导检测器
和100Ixl环形进样器(‰p)的离子谱仪。阴离子预分离
柱:直径3mmx150mm,用弱阴离子交换树脂装柱(Dionex);
阴离子分离柱:直径3mmx500mm,用弱阴离子交换树脂装
柱(Dionex);阴离子抑制柱:直径6mmx250mm,用阳离子交
换树脂装柱(Dionexo流动相为0.003mol/LNaHCOJ0.0024
mol/LNa2C03,流速为2.3mi/min。我们使用美国Dionex公司防御素
的DX-600型离子谱仪。采用EC,40淋洗液发生器,利用只
加水技术,以在线方式将去离子水转变成为高纯度的淋洗液,
可更换的EluGen瓶可以产生用于阴离子分析的氢氧化钾和
用于阳离子分析的甲磺酸。提高了保留时间的稳定性和分
离效果。
2.线性范围的测试:分别吸取标准储备液(26mgCm_1)25、
50、75、100、125、150,175、200Ixl,分别加水定容至25ml,其
浓度分别为650、1300、1950、2600、3250、3900、4550、5200
0.g/25
ml。以标准曲线的f:下弯曲点之间的直线部分确定为
线性范围。该方法的测定范围为650~5200斗g/25ml(5200
斗g/25
IIll浓度以上没有做)。
3.检出限的测试:连续测定lO次空白水溶液。其蜂面积
均值为0.013I.tS·rain。检出限为2.25“g,“,最低检出浓度
(以75L空气体积计)为0.75mrc'm3。
4.精密度和准确度的测试:lO份采样后滤膜,按样品测
定方法进行洗脱,合并洗脱液定容至500ml,测定样晶含量,
将洗脱液分为18份,分别加入标准储备液25、50、100斗l,平
行样6份。分别在1、2、3d测定,计算其加标回收率(%)和相
对标准偏差(RSDo由表1可见,RSD为1.26%~5.94%,平均
3.95%;样品加标回收率为96.6%~103.2%,平均99.1%。
表1精密度和准确度测试结果(0./25m1)
天数(d)本底浓度加人浓度检出浓度(互盐)相对标准偏差(%)回收率(%)125
5.洗脱效率的测试:10份李白滤膜分别加入26mg/mi的标准溶液25、50、100“l(浓度650、1300、2600o.g/25m1).自然干燥,放置过夜,洗脱并测得每份滤料的待测物量,计算其加标回收率及RSD。结果洗脱效率平均为98.2%。RSD为3.08%。
6.样品稳定性的测试:加标后的滤膜分别在室温、4℃冰箱密封放置,于当天及第5、7、14天测定,计算其加标同收率及RSD,见表2、表3。表3结果表明,样晶在室温下放置,采样后的滤膜应尽快分析,在室温下最多可保存5d;4℃冰箱放置第14天下降率为4.8%,说明样品在4℃冰箱放置至少可保存14d。
表2室温放置样品稳定性的测试结果(n=6,pg/25m1)表34℃冰箱放置样品稳定性测试结果(n=6,斗g/25m1)
7.干扰试验:人为加入水中常见的离子F一、CI一、S042一,观察加入离子与被测离子出峰时间及分离情况。与磺酸根离子保留时间相近的离子为FL,其保留时间为3.08min。与磺酸根离子可以完伞分离,不干扰测定结果,见图l。
-o.35.010.015.0
时间(rnin)
l:F-;2:SO州Hf;3:C1一
图1磺酸根离子的谱图
(中国疾病预防控制中心职业卫生与中毒控制所H慧芳老师及科室其他同志给予了大力支持和热情帮助,志谢)
(收稿H期:2009—01—20)
(本文编辑:杨德一)
工作场所空气中氨基磺酸铵的离子谱测定法
作者:关维俊, 白玉萍, 徐国卉, 庞淑兰, 陈刚
作者单位:华北煤炭医学院预防医学系,唐山,063000
刊名:
秸杆燃气炉
中华劳动卫生职业病杂志
英文刊名:CHINESE JOURNAL OF INDUSTRIAL HYGIENE AND OCCUPATIONAL DISEASES
年,卷(期):2010,28(2)
被引用次数:0次
1.期刊论文李意反相离子对谱法对两种新型苯磺酸类染料中间体的研究-分析试验室2004,23(8)
用Zorbax SB C18柱对2-氨基-4-氯-5-甲基苯磺酸和4-氨基-5-甲氧基-2-甲基苯磺酸两种新型染料中间体进行了反相离子对谱法的研究.以甲醇和2 mmol/L四丁基溴化铵,5 mmol/L磷酸二氢钠溶液为流动相,紫外检测波长215 nm.可在15 min内对这两种染料中间体分别进行杂质检测和纯度分析.线性范围均为0.2~2.0 μg,回归方程分别为Y=648.3+71.2ρ, r=0.9995; Y=177.3+65.0ρ, r=0.9994.该方法可用于对这两种染料中间体产品质量的监控及产品真伪的辨别.
2.外文期刊Corrie Weisensee Enhancing the Determination of Sulfonic Acids using Anion-Exchange
Chromatography with Post-Column Derivatization and Spectrometric Detection
Accurate determination of cysteic acid, homocysteic acid, and taurine in aqueous solution is essential in many analyses of biological and clinical applications. These sulfonic acids are difficult to be separated and determined using reversed phase chromatography and cation-exchange chromatography. In this research, an accurate and sensitive determination for the three sulfonic acids has been achieved using anion-exchange chromatography with post-column derivatization and spectrometric detection. This technique has outperformed the technique using suppressed conductivity detection. It has enormously enhanced the accuracy, detection limit, sensitivity, and linearity in the determination of these three sulfonic acids. This technique has demonstrated to be excellent for simultaneously determining cysteic acid, homocysteic acid, and taurine.
3.外文期刊Auger.J Fast narrow-bore HPLC-DAD analysis of biologically active thiosulfinates obtained
without solvent from wild Allium species.
4.外文期刊Raaschou-Nielsen.O Perfluorooctanoate and perfluorooctanesulfonate plasma levels and risk
内作of cancer in the general Danish population.
Perfluorooctanoate and perfluorooctanesulfonate are used in many industrial products and have been widely detected in human blood. Both chemicals are associated with tumor development in animal studies, but data on carcinogenic potential in humans are sparse. We investigated the association between plasma levels of perfluorooctanoate and perfluorooctanesulfonate and cancer risk within a prospective Danish cohort of participants with no previous cancer diagnosis at enrollment. From enrollment, between December 1, 1993, and May 31, 1997, and through July 1, 2006, we identified 713 participants with prostate cancer, 332 with bladder cancer, 128 with pancreatic cancer, and 67 with liver cancer in the entire cohort and we selected a comparison subcohort of 772. Plasma concentrations of perfluorooctanoate and perfluorooctanesulfonate were measured in each participant by use of high-pressure liquid chromatography coupled to tandem mass spectrometry. We found no clear differences in incidence rate ratios for these cancers in relation to plasma concentrations of perfluorooctanoate or perfluorooctanesulfonate. A 30%-40% increase in risk estimates for prostate cancer was observed for the three upper quartiles of perfluorooctanesulfonate concentration compared with the lowest
quartile (eg, for the lowest vs the fourth quartile, incidence rate ratio = 1.38, 95% confidence interval = 0.99 to 1.93). Plasma concentrations of perfluorooctanoate and perfluorooctanesulfonate in the ge
neral Danish population appear not to be associated with risk of prostate, bladder, pancreatic, or liver cancer.
5.学位论文张凌强力霉素生产废水处理与资源化研究2006
cnc真空吸盘怎么做强力霉素药品是目前应用较为广泛的抗生素药物之一。其工业废水产生于强力霉素生产的前期氯代、消除、氢化、置换的混合废液及洗涤废水。本文通过对强力霉素生产工艺调查及工业废水进行水质分析,确定了强力霉素工业废水的水质特点:强力霉素工业废水属于高浓度有机废水,酸度较低
,度深、臭味大、成份复杂,含有大量的生物难降解物质及生物毒性物质,废水的可生化性差。根据此特点,本文首先采用络合萃取的方法,对其中的主要污染物进行资源化回收研究;然后采用沉淀-吸附-混凝处理去除生物毒性物质,以提高废水的可生化性;最后采用生化法处理,实现达标排放。    根据强力霉素废水的特殊性,分析了主要污染物指标(CODCr,BOD5等);建立了气相谱法同时测定废水中甲醇、乙醇含量的方法;建立了同时测定废水中磺基水杨酸(SSA)与对甲基苯磺酸(PTSA)的紫外光谱法;考察了化学需氧量(CODCr)与有机物(SSA、PTSA、甲醇、乙醇)之间的关系,为采取相应的治理措施奠定了基础。
根据络合萃取对极性有机物稀溶液的分离具有高效性和高选择性的特点,本文选用了三烷基胺(7301)为络合剂,磺化煤油、正辛醇为稀释剂
,NaOH为反萃取剂,进行了萃取—反萃取实验。探讨了萃取体系的pH、油水比、萃取剂浓度、稀释剂浓度以及反萃取剂浓度、反萃温度对萃取效率的影响,确定了最佳的工艺条件。结果表明,控制油水比1∶1、废水pH2.0、络合萃取剂组成(体积比)为三烷基胺∶正辛醇∶磺化煤油=3∶3∶4时,通过三级萃取后,SSA总萃取率达到99.8%,PTSA总萃取率达到95.4%,CODCr总去除率达到92.8%;生化需氧量/化学需氧量(BOD5/CODCr)由原来的小于0.1提高至0.3。反萃使用25%的NaOH,控制油碱比为1∶1、反萃取温度40℃时,一次反萃取率接近100%。采用萃取—反萃取工艺处理该废水,不但有明显的环境效益,而且还可以回收磺酸类物质,取得良好的经济效益。
对络合萃取回收磺酸类物质后的强力霉素废水,采用沉淀-吸附-混凝联合工艺进行了处理研究。筛选出了最佳吸附剂、混凝剂、助凝剂,考察了其投加量、pH、反应时间等因素对处理效果的影响。研究表明:控制沉淀反应Ca/F质量比为2.0,反应时间为40min。选用粉煤灰作为吸附剂,其最佳用量为80g/L,适宜pH8左右,吸附时间80min。使用聚合氯化铝(PAC)作为混凝剂(最佳用量为450mg/L、适宜pH7.0~8.0),羟乙基田菁胶(ESG)作为助凝剂(最佳用量为15mg/L),220r/min的转速快速搅拌30s,然后以60r/min的转速慢速搅拌20min后,F-去除率达到99.9%,氟浓度降至10mg/L以下;CODCr去除率达到43.5%,进一步降低了有毒物质的含量;BOD5/CODCr由原来的0.3提高至0.4,提高了废水的可生化性,从而为后续的生化处理奠定了基础。
研究并分析了影响生化法处理沉淀-吸附-混凝后废水的主要因素,得到了利用高效活性污泥法去除废
猴子的B和人的B一样吗水中CODCr的最佳条件:温度为
20~35℃,pH7.0~8.0,溶解氧(DO)大于3.0mg/L,污泥浓度(MLSS)大于3.5g/L。在此条件下处理该废水22h,可使出水CODCr达到国家制药行业废水排放标准(GB8978-1996,CODCr≤300mg/L;BOD5≤150mg/L;SS≤200mg/L;F≤10mg/L),从而为进一步工程处理强力霉素废水提供技术参数。
处理后的灰渣可烧制成砖,不仅消除了废渣对环境造成的二次污染,其砖的强度、浸出毒性、材料放射性核素均达到了国家标准,可作为建筑材料使用。实现了以废治废、综合利用的目的。
conditions for lipophilicity assessment.
The chromatographic behavior of enalapril was investigated under different stationary and mobile phase conditions in an effort to unravel interferences in the underlying retention mechanism, which would affect its relation to octanol-water partitioning. Extrapolated retention factors, logk(w), were used as relevant chromatographic indices. The retention/pH profile was established and the peak split phenomenon, associated with cis/trans interconversion, was also monitored as a function of pH. The pH at maximum retention and minimum peak split occurrence was chosen for further investigation, so that the presence of zwitterionic structure was guaranteed and any effect of cis/trans interconversion could be ignored. Retention of zwitterionic enalapril was found to be very se
nsitive to mobile phase conditions in regard to organic modifier as well to the aqueous component. The use of morpholine-propanesulfonic acid (MOPS) as buffer and the presence of n-octanol as mobile phase additive proved critical factorsfor maximum suppression of secondary interactions. Nevertheless, the corresponding extrapolated retention factor was considerably larger than octanol-water logD value at the isoelectric point. However, logk(w) could be successfully converted to logD by means of a calibration equation established for ionized acidic compounds.
7.外文期刊Hayes.RN Validated HPLC/MS/MS assay for CI-1011 in rat plasma and a comparison with an
HPLC/UV assay.
A liquid chromatographic/mass spectrometric (LC/MS/MS) method to quantitate CI-1011 in rat plasma has been validated and compared to an LC/UV assay. The analyte and internal standard were isolated from the plasma matrix by using liquid/liquid extraction with diethyl ether. The ether layer was evaporated to dryness and the residue reconstituted in acetonitrile-water (70:30, v/v). A 2.1 x 150 mm x 5 microns Zorbax RX-C18 column with a mobile phase of acetonitrile-ammonium acetate (pH 8.0; 5 mM)-triethylamine
(70:30:0.03, v/v/v) delivered at a flow rate of 0.2 ml min-1 was used for chromatography. Analyte and internal standard ion chromatograms were obtained by operating the mass spectrometer in the negative ion multiple reaction monitoring mode to detect the presence of a precursor-product ion pair for both the analyte and the internal standard. Samples were introduced into the mass spectrometer using electrospray ionization. Retention times of CI-1011 and of the internal standard (IS), [13C6]CI-1011, were approximately 4.2 min. No peaks interfering with the quantitation of CI-1011 were observed throughout the validation process. Mean recoveries of CI-1011 from rat plasma ranged from 98.2 to 105%. The recovery of the IS was 100%. Assay precision for CI-1011, based on the percent relative standard deviation of replicate quality controls, was less than or equal to 5.60% with an accuracy of +/-
8.80%. The lower limit of quantitation for CI-1011 was 0.500 ng ml-1 for a 0.2-ml sample aliquot. CI-1011 is stable in rat plasma for 24 h at room temperature and for at least 34 days at -20 degrees C. This assay has been proven suitable for routine quantitation of CI-1011 in rat plasma at concentrations from 0.500 (100 pg on-column) to 500 ng ml-1. The applicability of this method to determine CI-1011 concentrations in rat plasma is reported in this manuscript. CI-1011 concentrations, in plasma samples from cholesterol- and chow-fed rats administered single daily oral doses of CI
8.外文期刊Takeshita.H Specific determination of linear Alkylbenzenesulfonates (LAS) in commercial
detergents and whole blood by high-performance liquid chromatography with solid-phase extraction.
This paper presents the extraction and analysis of linear alkylbenzenesulfonates (LAS) from whole blood using solid-phase extraction (SPE) together with high-performance liquid chromatography (HPLC). The sample was buffered with extraction solution and purified with Bakerbond C(18) SPE columns. The columns were washed, dried, and eluted with experimental optimized solvent systems. HPLC was performed using a Wakopak) WS AS-Aqua column (4.6 * 250-mm) and monitored at 228 nm using a UV detector. A mobile phase consisting of acetonitrile/water (60:40, v/v) and containing 1.2% (w/v) of sodium perchlorate was employed. Good separation was achieved for the five homologues of LAS (C(10) approximately C(14)) eluted at 6.85 and 13.79 min. The linearity range for this analysis was found to be from 10.0 to 100.0 ng/g and the limit of detection was 4.0-5.0 ng/g in blood for each homologue. The recovery of each homologue in blood ranged from 76 to 107%. The LAS in commercial detergents could be extracted and the homologues of C(10) approximately C(13) were detected. Blood samples of rats, which were administered a commercial detergent orally, were determined by the present method, and C(14) was used as an internal standard. The method was simple and reliable for the determination of LAS in blood samples and could be expected to appl
y to the forensic and clinical specimens.
9.外文期刊Fernandez.P Validated liquid chromatographic method for quantitative determination of
allicin in garlic powder and tablets.
In the present study, an RP high performance liquid chromatographic method was developed and validated for the determination of allicin in garlic powder and tablets. Chromatographic separation was carried out on an RP-18(e )column (125 mm x 4 mm), using a mobile phase, consisting of methanol-water (50:50 v/v), at a flow rate of 0.5 mL/min and UV detection at 220 nm. Ethylparaben was used as the internal standard. The assay was linear for allicin concentrations of 5.0-60.0 microg/mL. The RSD for precision was
<6.14%. The accuracy was above 89.11%. The detection and quantification limits were 0.27 and 0.81 microg/mL, respectively. This method was used to quantify allicin in garlic powder samples. The results showed that the method described here is useful for the determination of allicin in garlic powder and tablets.
10.外文期刊Lunte.CE Correlation of the capacity factor in vesicular electrokinetic chromatography
with the octanol:water partition coefficient for charged and neutral analytes.
PURPOSE: The aim of this study was to develop a method based upon electrokinetic chromatography (EKC) using oppositely charged surfactant vesicles as a buffer modifier to estimate hydrophobicity (log P) for a range of neutral and charged compounds. METHODS: Vesicles were formed from cetyltrimethylammonium bromide (CTAB) and sodium n-octyl sulfate (SOS). The size and polydispersity of the vesicles were characterized by electron microscopy, dynamic light scattering, and pulsed-field gradient NMR (PFG-NMR). PFG-NMR was also used to determine if ion-pairing between cationic analytes and free SOS monomer occurred. The CTAB/SOS vesicles were used as a buffer modifier in capillary electrophoresis (CE). The capacity factor (log k') was calculated by determining the mobility of the analytes both in the presence and absence of vesicles. Log k' was determined for 29 neutral and charged analytes. RESULTS; There was a linear relationship between the log of capacity factor (log k') and octanol/water partition coefficient (log P) for both neutral and basic species at pH 6.0, 7.3, and 10.2. This indicated that interaction between the cation and vesicle was dominated by hydrophobic forces. At pH 4.3, the log k' values for the least hydrophobic basic analytes were higher than expected, indicating that electrostatic attraction as well as hydrophobic forces contributed to the overall interaction between the cation and vesicle. Anionic compounds coul
d not be evaluated using this system. CONCLUSION: Vesicular electrokinetic chromatography (VEKC) using surfactant vesicles as buffer modifiers is a promising method for the estimation of hydrophobicity.
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