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气相色谱-质谱法测定化妆品中多种防腐剂 总被引:16,自引:0,他引:16
采用超声抽提法对化妆品中的苯甲醇、3-甲基-4-异丙基苯酚、对羟基苯甲酸丁酯和2-苄基-4-氯酚等18种防腐剂进行了气相色谱-质谱法(GC-MS)测定的研究。建立了一种简单、快速、准确测定化妆品中各种防腐剂的测定方法。进行了样品提取溶剂和超声提取时间选择以及线性、回收率、精密度试验。结果表明,该方法能够有效地提取化妆品(口红和香波)中的18种防腐剂,并可对其进行GC-MS分离和鉴定。18种防腐剂的平均回收率为91.66%-100.6%(n=7),相对标准偏差为0.46%-6.23%(n=7),最低检测限为 相似文献
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建立气相色谱-质谱法快速测定化妆品中甲基柏木酮、甲基柏木醚、壬酸3种香精香料的方法。样品用甲醇超声提取,经高速冷冻离心,上清液干燥脱水后经0.45 μm滤膜过滤,直接注入气相色谱-质谱仪进行测定,用选择离子和保留时间定性,外标法定量。甲基柏木酮、甲基柏木醚、壬酸在各自的质量浓度范围内与色谱峰面积成良好的线性关系,相关系数分别为0.9992,0.9991,0.9994,检出限分别为0.05,0.1,0.1 mg/kg。测定结果的相对标准偏差为2.1%~6.6%(n=5),样品加标回收率为91.5%~97.7%。该方法准确度和灵敏度高,样品用量少,前处理简单,可同时测定化妆品中3种香精香料。 相似文献
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气相色谱-质谱法测定化妆品中10种防腐剂 总被引:2,自引:0,他引:2
采用气相色谱-质谱法(GC-MS)同时测定化妆品中10种防腐剂含量。样品经甲醇超声提取,无水硫酸钠脱水后过滤进样检测。采用Agilent HP-5MS毛细管色谱柱(30m×0.25mm,0.25μm)分离,程序升温,分流进样进行测定。结果表明:17min内即可完成10种防腐剂的测定,各防腐剂的质量浓度均在5.00~100mg·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)为0.30~0.70ng。方法用于化妆品测定,加标回收率在96.5%~105%之间,测定值的相对标准偏差(n=6)在0.66%~3.2%之间。 相似文献
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防晒剂广泛应用于化妆品中,是目前化妆品监管的重点。建立了同时测定化妆品中13种防晒剂的气相色谱-质谱(GC-MS)方法。化妆品样品经二氯甲烷提取后,涡旋超声后稀释。采用程序升温模式,经HP-5ms毛细管色谱柱(30 m×250 μm×0.25 μm)在30 min内对13种防晒剂实现分离,经电子轰击(EI)源电离后采用选择离子监测模式(SIM)扫描测定,外标法定量。比较了6种常用有机溶剂的基质效应和平均回收率,二氯甲烷的基质效应弱,平均回收率较高。13种防晒剂在相应的线性范围内线性关系良好,相关系数均大于0.998,检出限(LOD, S/N=3)为0.04~0.63 mg/g,定量限(LOQ, S/N=10)为0.12~2.10 mg/g。实验选取了两种基质,在3个水平下验证方法的回收率和精密度,13种防晒剂在霜类基质中的加标回收率为88.7%~103.6%,相对标准偏差(RSD, n=6)为1.7%~4.9%,在乳类基质中的加标回收率为88.4%~102.3%, RSD(n=6)为1.2%~3.9%。美白类化妆品常添加防晒剂成分,为监管盲区,采用该方法检测了5批含有防晒剂的美白类化妆品,其所含5种防晒剂的含量为0.8%~5.2%,符合相关要求。该方法操作简单,灵敏度高,回收率好,测定的13种防晒剂均为我国《化妆品安全技术规范》2015版规定的常用的限用组分,可以用于各类化妆品中13种防晒剂的定性定量测定,为市场监管和实验室检测提供新的技术支持。 相似文献
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气相色谱-负化学源质谱法测定蜂蜜和奶粉中氯霉素残留量 总被引:8,自引:1,他引:8
研究了蜂蜜和奶粉中氯霉素残留量的气相色谱——质谱分析方法。将样品溶于水,其中的氯霉素残留物用乙酸乙酯提取,提取物用C18固相萃取柱净化,净化液再用乙酸乙酯反提取,经N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA) 1%三甲基氯硅烷(TMCS)衍生后,用配有负化学源质谱检测器的气相色谱仪测定。当添加水平为0.1~10μg/kg时,回收率为80.4%~95.3%,相对标准偏差为9.3%~18.1%。 相似文献
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吕琼芳彭敏梁惠明黄少宏 《化学分析计量》2023,(1):45-49
建立气相色谱-质谱法同时测定化妆品中斑蝥素和氮芥的含量。以色谱纯三氯甲烷为溶剂提取化妆品中的斑蝥素和氮芥两种组分,用气相色谱-质谱(GC-MS)法进行分析,各目标组分均能有效分离,且色谱峰形良好。斑蝥素和氮芥在质量浓度0.5~10μg/mL范围内线性良好,线性相关系数均为0.998,平均加标回收率分别为102.6%和115.7%。测定结果的相对标准偏差分别为1.2%和2.1%(n=6)。该方法适用于化妆品中斑蝥素和氮芥两种禁用组分同时测定。 相似文献
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建立了一种用于各种动物源性食品中氯霉素残留量的气相色谱-负化学离子源质谱(GC-MS/NCI)检测方法。以氘代氯霉素(D5-CAP)为内标物,用乙酸乙酯对各类样品中的氯霉素进行提取,用正己烷和40 g/L NaCl溶液液液分配除脂肪,基质复杂的样品再用Oasi HLB固相萃取柱净化,经硅烷化衍生后由GC-MS/NCI在选择离子监测模式下进行测定。多数样品在0.2,0.5,1.0μg/kg3个添加水平下氯霉素的回收率处于87.8%和107.0%之间,相对标准偏差(RSD)不大于8.5%。方法在2.0~80.0μg/L范围内有良好的线性关系,基质复杂样品中氯霉素残留的检出限达到0.1μg/kg,基质简单样品的检测限可达0.05μg/kg。方法适合各种动物源性食品中氯霉素残留量的确证分析。 相似文献
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Although chlorinated paraffins (CP) are produced in large amounts (300 000 tonnes per year), little is known about their occurrence in the environment due to the lack of specific and sensitive analytical methods. The present paper describes the GC/MS analysis of different CP's using capillary gas chromatography with on-column injection and negative ion chemical ionization (NCI) mass spectrometry. Chromatographic resolution of groups of isomers and homologues was obtained. The chromatograms and mass spectra are discussed. The suitability of this method for trace analysis of a CP sample using multiple ion detection (MID) is described. 相似文献
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林蛙油中农药残留的GC-MS/MS检测方法 总被引:3,自引:0,他引:3
首次建立了林蛙油中15种农药(p,p′DDE,O,p′-DDD,o p′-DDT,p,p′-DDT,BHC(α、β、γ、δ),异丙威,甲拌磷,六氯苯,百菌清,皮蝇磷,倍硫磷,甲氰菊酯)的GC—MS/MS残留检测方法。样品用乙酸乙酯提取、Florisil层析柱净化后,经GC—MS/MS检测,用外标法定量。15种农药在0.050~10.0mg/L范围内,线性关系良好,相关系数r≥0.996。当添加量在0.050—2.00mg/kg间,平均加标回收率为81%~117%,RSD为2.4%-18.2%,方法的检出限为0.050mg/kg。该方法准确、灵敏,适用于农药残留的分析。 相似文献
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采用电子轰击(EI)和负化学(NCI)离子源两种离子源技术气相色谱-质谱联用法(GC-MS)测定了蔬菜中10类除草剂的残留量, 并对两种方法进行了比较. 样品经乙腈提取后, 用PSA固相萃取柱净化, 由气相色谱-质谱联用EI或NCI技术进行定量和定性分析. 对含电负性强的除草剂分析, NCI灵敏度高, 在10 ng/g, 20 ng/g和40 ng/g 3个添加水平下的方法回收率为70%~115%, RSD为1.7%~10.1%, 两种离子源技术可以互相补充用于准确检测蔬菜中多类除草剂. 相似文献
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GC determination of N-nitrosamines by supersonic molecular beam MS equipped with triple quadrupole analyzer, GC/SMB/QQQ/MS 总被引:1,自引:0,他引:1
The determination of 14 N-nitrosamines by a supersonic molecular beam electron ionization mass spectrometer equipped with triple quadruple analyzer, GC/SMB/EI/QQQ/MS is presented. The supersonic molecular beam electron ionization ion source allows the elucidation of the molecular ion of 13 out of the 14 examined nitrosamines (except for diphenylnitrosamine which was degraded before the analysis). It was possible to use the molecular ions of all the nitrosamines as the parent ions for multiple reactions monitoring mode, which in turn allows significant increase of specificity and lowering of the method limit of detection of the higher molecular weight nitrosamines. The instrumental LOD for different N-nitrosamines was 1–5 pg injection−1. The proposed method was exemplified by analysis of N-nitrosamines and N-nitrosatables in rubber teats according to the British Standard BS EN 12868:1999. 相似文献
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Jianbing Wu Linyao Chen Peipei Mao Yanbin Lu Huizhong Wang 《Journal of separation science》2012,35(24):3586-3592
An effective analytical protocol using graphene‐based SPE coupled with HPLC‐MS/MS for determination of chloramphenicol (CAP) in aquatic products has been developed. In the present work, graphene was evaluated as SPE sorbents for the analytes enrichment and clean up. The target analytes were quantified by a triple‐quadrupole linear ion trap MS in multiple‐reaction monitoring mode. In addition, the proposed method was validated according to Commission Decision 2002/657/EC. The calibration curve was linear over the range of 0.5–100 ng/mL. The mean values of RSD of intra‐ and interday ranging from 1.48 to 4.29% and from 3.25 to 7.42% were obtained, respectively. In the three fortified levels, the recoveries of CAP ranging from 92.3 to 103.4% with RSDs ≤ 5.58% were obtained. The proposed method has been successfully applied to the analysis of CAP in several aquatic product samples, indicating that graphene was a potential SPE sorbent for the enrichment of trace residues in food samples. 相似文献
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Flavor samples are complex mixtures with components of sometimes very similar chemical behavior (e.g. isomeres). As an approach towards their characterization an integrated analytical method on the basis of capillary gas-chromatography (HRGC) was applied consisting of two molecular specific techniques for component-identification in unknown samples: GC-FTIRS (GC-Fourier transform infrared spectrometry) and GC-MS (GC-mass spectrometry).In addition GC-retention indices-from simultaneous GC on two columns (nonpolar/polar) —were stored in a database for routine retrieval and quantitative monitoring. To correlate this information with sensory perception sniffing chromatograms were generated with the human nose as a high performance detector.Because of the high information contents of GC-FTIR spectra in this field a small but specific vapor-phase-FTIR flavor library was accumulated, which dramatically improved the fast identification power of GC-FTIRS alone. 相似文献
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Fabio Busico Gabriella Moretti Giampaolo P. Cartoni Felice Rosati 《Journal of separation science》1992,15(2):94-98
GC-MS with negative ion chemical ionization has been used to detect anabolic estrogens (diethylstilbestrol, dienestrol, hexestrol, and 17β- and 17α-estradiol) in bovine muscle tissue. After hydrolysis and extraction, purification by column chromatography, and derivatization, the detection limit for the estrogens is better than 0.1 ppb. 相似文献