阿魏酰落叶松脂对照品

[align=center][font='times new roman'][size=20px]基于[url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]液质[/color][/url]联[/size][/font][font='times new roman'][size=20px]用仪[/size][/font][font='times new roman'][size=20px]([url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]LC-MS[/color][/url]/MS)[/size][/font][font='times new roman'][size=20px]测定农作物中[/size][/font][font='times new roman'][size=20px]松柏醇、松脂醇、落叶松脂素[/size][/font][/align][align=center][font='times new roman']仪莹[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][font='times new roman']，[/font][font='times new roman']孙莹璐[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][font='times new roman']，[/font][font='times new roman']张丽娜[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][/align][align=center][font='times new roman'](1.[/font][font='times new roman']中国农业科学院[/font][font='times new roman'] [/font][font='times new roman']作物科学研究所[/font][font='times new roman'] [/font][font='times new roman']重大平台中心，北京[/font][font='times new roman'] 100089[/font][font='times new roman']；[/font][font='times new roman']2.[/font][font='times new roman']中国仪器仪表学会科学仪器设备验证评价中心（生命科学站），北京[/font][font='times new roman'] 100089)[/font][/align][font='times new roman']摘要[/font][font='times new roman']: [/font][font='times new roman']用超高效[url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相色谱[/color][/url][/font][font='times new roman']-[/font][font='times new roman']串联三重四[/font][font='times new roman']极[/font][font='times new roman']杆质谱法[/font][font='times new roman'](UP[url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]LC-MS[/color][/url]/MS)[/font][font='times new roman']检测农作物中的[/font][font='times new roman']松柏醇（[/font][font='times new roman']CA[/font][font='times new roman']）[/font][font='times new roman']、[/font][font='times new roman']松脂醇（[/font][font='times new roman']Pin[/font][font='times new roman']）、落叶松脂素（[/font][font='times new roman']Lar[/font][font='times new roman']）[/font][font='times new roman']，色谱柱为[/font][font='times new roman']Agilent SB C18 RRHD[/font][font='times new roman']，[/font][font='times new roman']检测柱温为[/font][font='times new roman']40[/font][font='times new roman']℃[/font][font='times new roman']，[/font][font='times new roman']初始[/font][font='times new roman']流动相为乙腈[/font][font='times new roman']∶[/font][font='times new roman']水[/font][font='times new roman']=4[/font][font='times new roman']∶[/font][font='times new roman']1[/font][font='times new roman']，按[/font][font='times new roman']5mM[/font][font='times new roman']的量加乙酸铵，检测流速为[/font][font='times new roman']0.3mL/min[/font][font='times new roman']，其检出限分别为[/font][font='times new roman']1.25~ 5. 10 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']，定量[/font][font='times new roman']限分别[/font][font='times new roman']为[/font][font='times new roman']3. 75~ 15. 60 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']，满足农作物中[/font][font='times new roman']CA[/font][font='times new roman']、[/font][font='times new roman']Pin[/font][font='times new roman']和[/font][font='times new roman']Lar[/font][font='times new roman']同时检测的要求。[/font][align=left][font='times new roman']关键词：[/font][font='times new roman']超高效[url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相色谱[/color][/url][/font][font='times new roman']-[/font][font='times new roman']串联质谱；[/font][font='times new roman']松柏醇[/font][font='times new roman']；[/font][font='times new roman']松脂醇[/font][font='times new roman']；[/font][font='times new roman']落叶松脂素；[/font][font='times new roman']农作物[/font][/align][align=center][font='times new roman'][size=18px][color=#666666]Determination of [/color][/size][/font][font='times new roman'][size=18px][color=#666666]CA[/color][/size][/font][font='times new roman'][size=18px][color=#666666], [/color][/size][/font][font='times new roman'][size=18px][color=#666666]Pin [/color][/size][/font][font='times new roman'][size=18px][color=#666666]and[/color][/size][/font][font='times new roman'][size=18px][color=#666666] Lar[/color][/size][/font][font='times new roman'][size=18px][color=#666666] in crops based on [url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]LC-MS[/color][/url]/MS[/color][/size][/font][/align][align=center][font='times new roman']Y[/font][font='times new roman']i[/font][font='times new roman'] Ying[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][font='times new roman'] ,[/font][font='times new roman'][sup][size=13px] [/size][/sup][/font][font='times new roman']S[/font][font='times new roman']un[/font][font='times new roman'] Yinglu[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][font='times new roman'],[/font][font='times new roman']Z[/font][font='times new roman']hang[/font][font='times new roman'] Lina[/font][font='times new roman'][sup][size=13px]12[/size][/sup][/font][/align][align=center][font='times new roman'][size=12px]([/size][/font][font='times new roman'][size=12px]1.Major[/size][/font][font='times new roman'][size=12px] Platform Center, Institute of Crop Sciences, Chinese Academy of Agricultural Sciences, Beijing 100089, China 2. Scientific Instruments and Equipment Verification and Evaluation Center of China Instruments and Apparatus Society (Bioscience Station))[/size][/font][/align][font='times new roman']Abstract[/font][font='times new roman']：[/font][font='times new roman']Ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry (UP[url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]LC-MS[/color][/url]/MS) was used to detect [/font][font='times new roman']CA, Pin[/font][font='times new roman'] and [/font][font='times new roman']Lar[/font][font='times new roman'] in crops. The chromatographic column was Waters [/font][font='times new roman']Acquity[/font][font='times new roman'] [/font][font='times new roman']Agilent SB C18 RRHD[/font][font='times new roman'], the temperature of the detection column was [/font][font='times new roman']40[/font][font='times new roman']℃, the mobile phase consisted of [/font][font='times new roman']acetonitrile[/font][font='times new roman']:[/font][font='times new roman']water[/font][font='times new roman'] =4[/font][font='times new roman']:[/font][font='times new roman']1, and [/font][font='times new roman']5mM[/font][font='times new roman'] ammonium acetate was added. The detection [/font][font='times new roman']flow [/font][font='times new roman']rate was 0.3[/font][font='times new roman'] [/font][font='times new roman']mL/min, the detection limit[/font][font='times new roman']s[/font][font='times new roman'] w[/font][font='times new roman']ere[/font][font='times new roman'] 1.25-5.10 [/font][font='times new roman']μg[/font][font='times new roman']/L, [/font][font='times new roman']and [/font][font='times new roman']the quantification limit[/font][font='times new roman']s[/font][font='times new roman'] w[/font][font='times new roman']ere[/font][font='times new roman'] 3.75-15.60 [/font][font='times new roman']μg[/font][font='times new roman']/L, respectively[/font][font='times new roman'],[/font][font='times new roman'] [/font][font='times new roman']which satisfied t[/font][font='times new roman']he requirements [/font][font='times new roman']of[/font][font='times new roman'] simultaneous detection of T6P and Tre in crops.[/font][align=left][font='times new roman']Keywords:[/font][font='times new roman'] U[/font][font='times new roman']PLC[/font][font='times new roman']-MS/MS [/font][font='times new roman']CA[/font][font='times new roman'] [/font][font='times new roman']Pin[/font][font='times new roman'] [/font][font='times new roman']Lar [/font][font='times new roman']crops [/font][/align][font='times new roman'][size=18px]1 [/size][/font][font='times new roman'][size=18px]引言[/size][/font][font='times new roman']自[/font][font='times new roman']1997[/font][font='times new roman']年[/font][font='times new roman']Lewis[/font][font='times new roman']等首次提出[/font][font='times new roman']DIR[/font][font='times new roman']蛋白广泛存在于植物体内，参与并[/font][font='times new roman']指导木脂素[/font][font='times new roman']生物合成过程中位置的选择和立体选择，这类具有[/font][font='times new roman']dirigent[/font][font='times new roman']结构域的蛋白就引起了科学家的广泛关[/font][font='times new roman']注。为了[/font][font='times new roman']了解木脂素[/font][font='times new roman']在不同农作物组织中含量的差异，我们通过[/font][font='times new roman']HP[url=https://insevent.instrument.com.cn/t/Yp][color=#3333ff]LC-MS[/color][/url]/MS[/font][font='times new roman']平台[/font][font='times new roman']对木脂素[/font][font='times new roman']代谢途径中的母核化合物[/font][font='times new roman']CA[/font][font='times new roman']，[/font][font='times new roman']Pin[/font][font='times new roman']和[/font][font='times new roman']Lar[/font][font='times new roman']进行含量测定[/font][font='times new roman'][sup][size=13px][1,2][/size][/sup][/font][font='times new roman']。[/font][font='times new roman'][size=18px]2 [/size][/font][font='times new roman'][size=18px]材料和方法[/size][/font][font='times new roman']仪器与试剂：[/font][font='times new roman']谱育[/font][font='times new roman']EXPEC5210[/font][font='times new roman']三[/font][font='times new roman']重四[/font][font='times new roman']极[/font][font='times new roman']杆[url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相色谱[/color][/url]联用仪（[/font][font='times new roman']UPLC5210[/font][font='times new roman']二[/font][font='times new roman']元高压输液泵、自动进样器、[/font][font='times new roman']柱温箱[/font][font='times new roman']、质谱仪）、电子天平[/font][font='times new roman'](BSA224S[/font][font='times new roman']型，赛多利斯科学仪器有限公司产品[/font][font='times new roman']),KQ-250E[/font][font='times new roman']型超声波清洗器[/font][font='times new roman'] ([/font][font='times new roman']昆山禾创超声[/font][font='times new roman']仪器有限公司产品[/font][font='times new roman'])[/font][font='times new roman']，[/font][font='times new roman']PICO17[/font][font='times new roman']型离心机[/font][font='times new roman']([/font][font='times new roman']美国赛默飞公司产品[/font][font='times new roman'])[/font][font='times new roman']。[/font][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455540531_1340_5708872_3.jpeg[/img][/align][font='times new roman']乙腈[/font][font='times new roman']([/font][font='times new roman']色谱纯[/font][font='times new roman'],[/font][font='times new roman']美国赛默飞公司产品[/font][font='times new roman'])[/font][font='times new roman']，乙酸铵[/font][font='times new roman']([/font][font='times new roman']纯度[/font][font='times new roman']≥98[/font][font='times new roman']％，德国[/font][font='times new roman']CNW [/font][font='times new roman']公司产品[/font][font='times new roman'])[/font][font='times new roman']。[/font][font='times new roman'] T6P[/font][font='times new roman']和[/font][font='times new roman']Tre[/font][font='times new roman']购[/font][font='times new roman']sigma-[/font][font='times new roman']aldrich[/font][font='times new roman']贸易有限公司，质谱用水为屈臣氏蒸馏水。[/font][font='times new roman']分析条件：色谱柱[/font][font='times new roman']:Agilent SB C18 RRHD Column (100 mm×2.1 mm,1.8 [/font][font='times new roman']μm[/font][font='times new roman'])[/font][font='times new roman']，[/font][font='times new roman']柱温[/font][font='times new roman']40 ℃[/font][font='times new roman']，进样体积[/font][font='times new roman']5 [/font][font='times new roman']μl[/font][font='times new roman']，流动相[/font][font='times new roman']:A:[/font][font='times new roman']乙腈[/font][font='times new roman'] B:5 mM[/font][font='times new roman']乙酸铵[/font][font='times new roman']-[/font][font='times new roman']水，流速[/font][font='times new roman']0.3ml/min[/font][align=center][font='times new roman'][color=#666666]0min [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666] 20A%[/color][/font][/align][align=center][font='times new roman'][color=#666666]1 [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666] 20A%[/color][/font][/align][align=center][font='times new roman'][color=#666666]5 [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666] 80A%[/color][/font][/align][align=center][font='times new roman'][color=#666666]5.1 [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]20A%[/color][/font][/align][align=center][font='times new roman'][color=#666666]7 [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666] 20A%[/color][/font][/align][font='times new roman']离子源[/font][font='times new roman']:[/font][font='times new roman']电喷雾离子源；扫描方式[/font][font='times new roman']:[/font][font='times new roman']负离子切换扫描；检测方式：质谱多反应监测[/font][font='times new roman'](MRM)[/font][font='times new roman'][sup][size=13px] [3][/size][/sup][/font][font='times new roman']；优化的质谱条件见表[/font][font='times new roman']1[/font][font='times new roman']。[/font][align=center][font='times new roman'][size=12px][color=#666666]表[/color][/size][/font][font='times new roman'][size=12px][color=#666666]1[/color][/size][/font][font='times new roman'][size=12px][color=#666666] [/color][/size][/font][font='times new roman'][size=12px][color=#666666] Lar[/color][/size][/font][font='times new roman'][size=12px][color=#666666]和[/color][/size][/font][font='times new roman'][size=12px][color=#666666]CA[/color][/size][/font][font='times new roman'][size=12px][color=#666666]、[/color][/size][/font][font='times new roman'][size=12px][color=#666666]Pin[/color][/size][/font][font='times new roman'][size=12px][color=#666666]的质谱多反应检测质谱参数[/color][/size][/font][/align][table][tr][td][font='times new roman'][color=#666666]化合物[/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]母离子（[/color][/font][font='times new roman'][color=#666666]m/z) [/color][/font][font='times new roman'][color=#666666]子离子（[/color][/font][font='times new roman'][color=#666666]m/z) [/color][/font][font='times new roman'][color=#666666]锥孔电压[/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]碰撞能[/color][/font][font='times new roman'][color=#666666] [/color][/font][/td][/tr][tr][td][font='times new roman'][color=#666666]Lar [/color][/font][font='times new roman'] 359 329.1 50 [/font][font='times new roman'] [/font][font='times new roman'] 10[/font][/td][/tr][tr][td][font='times new roman'][color=#666666]CA [/color][/font][font='times new roman'][sub][size=13px] [/size][/sub][/font][font='times new roman'] 179.2 146[/font][font='times new roman']、[/font][font='times new roman']164 [/font][font='times new roman'] [/font][font='times new roman'] 50 [/font][font='times new roman'] [/font][font='times new roman'] 15[/font][/td][/tr][tr][td][font='times new roman'][color=#666666]Pin 357 151[/color][/font][font='times new roman'][color=#666666]、[/color][/font][font='times new roman'][color=#666666]136.1 50 [/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666] 20[/color][/font][/td][/tr][/table][font='times new roman'][size=18px]3 [/size][/font][font='times new roman'][size=18px]结果与分析[/size][/font][font='times new roman'][size=16px]3.1[/size][/font][font='times new roman'][size=16px]线性范围与检出限[/size][/font][font='times new roman']Agilent SB C18 RRHD[/font][font='times new roman']色谱柱检测时，[/font][font='times new roman']Lar[/font][font='times new roman']的质量浓度为[/font][font='times new roman']7.25 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']14.5 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']72.5 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']145 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']290 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']725 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']1450 [/font][font='times new roman']μg[/font][font='times new roman']/L, CA[/font][font='times new roman']的质量浓度为[/font][font='times new roman']8.65 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']17.3 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']43.25 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']86.5 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']173 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman'] 346 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']865 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']1730 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']，[/font][font='times new roman']Pin[/font][font='times new roman']的质量浓度为[/font][font='times new roman']8.23 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']16.46 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']82.3 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']164.6 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']329.2 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']823 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']、[/font][font='times new roman']1646 [/font][font='times new roman']μg[/font][font='times new roman']/L[/font][font='times new roman']；按照优化后的色谱条件对每个点重复测定[/font][font='times new roman']3[/font][font='times new roman']次。以质量浓度为横坐标，以峰面积为纵坐标，绘制标准曲线，以标准曲线的第一个和最后一个点的质量浓度作为线性范围。[/font][font='times new roman']不同浓度梯度的[/font][font='times new roman']Lar[/font][font='times new roman']、[/font][font='times new roman']CA[/font][font='times new roman']和[/font][font='times new roman']Pin[/font][font='times new roman']通过[/font][font='times new roman']C18[/font][font='times new roman']柱时在线性范围内呈现良好的线性关系；系数均在[/font][font='times new roman']0. 99 [/font][font='times new roman']以上，均符合实际分析的要求[/font][font='times new roman'][sup][size=13px][[/size][/sup][/font][font='times new roman'][sup][size=13px]4[/size][/sup][/font][font='times new roman'][sup][size=13px]][/size][/sup][/font][font='times new roman']。[/font][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455542574_4489_5708872_3.jpg[/img][/align][align=center][font='times new roman'][size=12px][color=#000000]图[/color][/size][/font][font='times new roman'][size=12px][color=#000000]1 [/color][/size][/font][font='times new roman'][size=12px][color=#000000]Lar[/color][/size][/font][font='times new roman'][size=12px][color=#000000]标准曲线[/color][/size][/font][/align][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455544692_9457_5708872_3.jpg[/img][/align][align=center][font='times new roman'][size=12px][color=#000000]图[/color][/size][/font][font='times new roman'][size=12px][color=#000000]2 [/color][/size][/font][font='times new roman'][size=12px][color=#000000]CA[/color][/size][/font][font='times new roman'][size=12px][color=#000000]标准曲线[/color][/size][/font][/align][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455545568_5903_5708872_3.jpg[/img][/align][align=center][font='times new roman'][size=12px][color=#000000]图[/color][/size][/font][font='times new roman'][size=12px][color=#000000]3 Pin[/color][/size][/font][font='times new roman'][size=12px][color=#000000]标准曲线[/color][/size][/font][/align][align=center][font='times new roman'][size=12px][color=#000000]表[/color][/size][/font][font='times new roman'][size=12px][color=#000000]2 [/color][/size][/font][font='times new roman'][size=12px][color=#000000] [/color][/size][/font][font='times new roman'][size=12px][color=#000000]Lar[/color][/size][/font][font='times new roman'][size=12px][color=#000000]、[/color][/size][/font][font='times new roman'][size=12px][color=#000000]CA[/color][/size][/font][font='times new roman'][size=12px][color=#000000]和[/color][/size][/font][font='times new roman'][size=12px][color=#000000]Pin[/color][/size][/font][font='times new roman'][size=12px][color=#000000]标准曲线、线性范围、决定系数、检出限和定量限[/color][/size][/font][/align][table][tr][td][font='times new roman'][color=#666666]化合物[/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]标准曲线方程[/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]线性范围[/color][/font][font='times new roman'][color=#666666]([/color][/font][font='times new roman'][color=#666666]μg[/color][/font][font='times new roman'][color=#666666]/L) [/color][/font][font='times new roman'][color=#666666]相关系数[/color][/font][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][color=#666666]检出限[/color][/font][font='times new roman'][color=#666666]([/color][/font][font='times new roman'][color=#666666]μg[/color][/font][font='times new roman'][color=#666666]/L) [/color][/font][font='times new roman'][color=#666666]定量限[/color][/font][font='times new roman'][color=#666666]([/color][/font][font='times new roman'][color=#666666]μg[/color][/font][font='times new roman'][color=#666666]/L) [/color][/font][/td][/tr][tr][td][font='times new roman'][color=#666666]Lar y[/color][/font][font='times new roman'][color=#666666]＝[/color][/font][font='times new roman'][color=#666666]422.9818x 7.25-1450 0.9996 1.25 3.75[/color][/font][/td][/tr][tr][td][font='times new roman'][color=#666666]CA y[/color][/font][font='times new roman'][color=#666666]＝[/color][/font][font='times new roman'][color=#666666]33.6037x 8.65- 1730 0.9996 5.10 15.60[/color][/font][/td][/tr][tr][td][font='times new roman'][color=#666666]Pin y[/color][/font][font='times new roman'][color=#666666]＝[/color][/font][font='times new roman'][color=#666666]9433.8945x 8.23- 1646 0.9998 3.59 10.77[/color][/font][/td][/tr][/table][font='times new roman'][size=16px]3.[/size][/font][font='times new roman'][size=16px]2[/size][/font][font='times new roman'][size=16px]实际样品的测定[/size][/font][font='times new roman']用建立的方法测定[/font][font='times new roman']40[/font][font='times new roman']份小麦类样品，部分样品的色谱图如图[/font][font='times new roman']4[/font][font='times new roman']所示。[/font][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455547572_5306_5708872_3.jpeg[/img][/align][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455549420_9726_5708872_3.jpeg[/img][font='times new roman'][color=#666666] [/color][/font][font='times new roman'][size=12px][color=#000000]图[/color][/size][/font][font='times new roman'][size=12px][color=#000000]4[/color][/size][/font][font='times new roman'][size=12px][color=#000000] [/color][/size][/font][font='times new roman'][size=12px][color=#000000]小麦叶片中[/color][/size][/font][font='times new roman'][size=12px][color=#000000]Lar[/color][/size][/font][font='times new roman'][size=12px][color=#000000]、[/color][/size][/font][font='times new roman'][size=12px][color=#000000]CA[/color][/size][/font][font='times new roman'][size=12px][color=#000000]和[/color][/size][/font][font='times new roman'][size=12px][color=#000000]Pin[/color][/size][/font][font='times new roman'][size=12px][color=#000000]的色谱图[/color][/size][/font][/align][font='times new roman']且同一批次样品[/font][font='times new roman']3[/font][font='times new roman']次平行[/font][font='times new roman']样得到[/font][font='times new roman']T6P[/font][font='times new roman']和[/font][font='times new roman']Tre[/font][font='times new roman']的[/font][font='times new roman']RSD [/font][font='times new roman']值小于[/font][font='times new roman']3%[/font][font='times new roman']，如表[/font][font='times new roman']3[/font][font='times new roman']所示，说明前处理方法可行，仪器的稳定性良好[/font][font='times new roman'][sup][size=13px][[/size][/sup][/font][font='times new roman'][sup][size=13px]5][/size][/sup][/font][font='times new roman']。[/font][align=center][img]https://ng1.17img.cn/bbsfiles/images/2023/10/202310301455551095_7818_5708872_3.png[/img][/align][align=center][font='times new roman'][size=12px][color=#000000]表[/color][/size][/font][font='times new roman'][size=12px][color=#000000]3[/color][/size][/font][font='times new roman'][size=12px][color=#000000] [/color][/size][/font][font='times new roman'][size=12px][color=#000000]小麦叶片中[/color][/size][/font][font='times new roman'][size=12px][color=#000000]Lar[/color][/size][/font][font='times new roman'][size=12px][color=#000000]、[/color][/size][/font][font='times new roman'][size=12px][color=#000000]CA[/color][/size][/font][font='times new roman'][size=12px][color=#000000]和[/color][/size][/font][font='times new roman'][size=12px][color=#000000]Pin[/color][/size][/font][font='times new roman'][size=12px][color=#000000]的测定值[/color][/size][/font][/align][font='times new roman']分别对小麦[/font][font='times new roman']不同组织的样本[/font][font='times new roman']进行前处理提取实验，前处理方法简便可行，仪器性能可靠，满足对样品中[/font][font='times new roman']松柏醇、松脂醇、落叶松脂素[/font][font='times new roman']的检测。[/font][font='times new roman']参考文献[/font][font='times new roman'][1] [/font][font='times new roman']周海旭[/font][font='times new roman']. [/font][font='times new roman']樟树[/font][font='times new roman']叶中木脂素[/font][font='times new roman']提取分离及其生物活性研究[/font][font='times new roman'][D]. 2017.[/font][font='times new roman'][2] [/font][font='times new roman']戴清源[/font][font='times new roman'],[/font][font='times new roman']朱秀灵[/font][font='times new roman'],[/font][font='times new roman']刘皓[/font][font='times new roman']. [/font][font='times new roman']芝麻木脂素[/font][font='times new roman']及其生物活性研究进展[/font][font='times new roman'][J]. [/font][font='times new roman']农产品加工[/font][font='times new roman'].[/font][font='times new roman']学刊[/font][font='times new roman'], 2012, (1[/font][font='times new roman']期[/font][font='times new roman']):16-21. [/font][font='times new roman'][3] Du, [/font][font='times new roman']Bingyuan[/font][font='times new roman'], et al. [/font][font='times new roman']Phillygenin[/font][font='times new roman'] exhibits anti-inflammatory activity through modulating multiple cellular behaviors of mouse lymphocytes[J]. Immunopharmacology and immunotoxicology, 2019, 41(1): 76-85.[/font][font='times new roman'][4] Murata, Jun, et al. Oxidative rearrangement of (+)-[/font][font='times new roman']sesamin[/font][font='times new roman'] by CYP92B14 co-generates twin dietary lignans in sesame[J]. Nature communications, 2017, 8(1): 1-10.[/font][font='times new roman'][5] Hano, C, et al. [/font][font='times new roman']Pinoresinol-lariciresinol[/font][font='times new roman'] reductase gene expression and [/font][font='times new roman']secoisolariciresinol[/font][font='times new roman'] [/font][font='times new roman']diglucoside[/font][font='times new roman'] accumulation in developing flax (Linum [/font][font='times new roman']usitatissimum[/font][font='times new roman']) seeds[J]. Planta, 2016, 224(6): 1291-1301.[/font]

[align=center][size=24px][b]松脂酸（松香酸）测定方法[/b][/size][/align] 松香酸用于发酵工业，并且可用作肥皂和造纸工业的填料。松香酸为三环二萜类化合物。在含水乙醇中得单斜片状结晶。熔点172～175℃，旋光度-102°(无水乙醇)。不溶于水，溶于乙醇、苯、氯仿、乙醚、丙酮、二硫化碳以及稀氢氧化钠水溶液。为天然松香树脂的主要成分。本测定方法是建立松香中松脂酸测定，液体原药松脂酸铜中松脂酸测定；文献报道，[url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相色谱[/color][/url]法测定松脂酸铜需要加入盐酸，[font=宋体]将松脂酸铜衍生转化为松脂酸，图[/font][font='Times New Roman','serif']1[/font][font=宋体]列出了其可能的转化途径，确定松脂酸铜实际测定对象为松脂酸。厂家送过来的原药是盐酸处理过的所以我们直接检测就行。[/font][align=center][img=,589,168]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150859397658_4592_3963412_3.jpg!w589x168.jpg[/img][/align][align=center][b][font=宋体]图[/font][font='Times New Roman','serif']1 [/font][/b][font=宋体][b]松脂酸铜转化为松脂酸[/b][/font][/align][align=left][b]实验方法[/b][/align][align=left][/align][align=left][font='Times New Roman','serif']1[/font][font=宋体]试剂：乙腈（色谱级），磷酸（分析纯）；盐酸分析纯[/font][font=&] [font='Times New Roman','serif']2[/font][font=宋体][url=https://insevent.instrument.com.cn/t/5p][color=#3333ff]液相[/color][/url]条件：[/font][font='Times New Roman','serif']LC-20AT [/font][font=宋体]波长：[/font][font='Times New Roman','serif']245nm [/font][font=宋体]；进样量：[/font][font='Times New Roman','serif']5μL[/font][font=宋体]色谱柱型号：[/font][font='Times New Roman','serif']Agilent Eclipse XDB-C18(2.1 mm×100mm, 2.7 μm), [/font][font=宋体]柱温：[/font][font='Times New Roman','serif']30.5 [/font][font=宋体]℃，流动相条件如表[/font][font='Times New Roman','serif']1[/font][font=宋体]：[/font][/font][/align][align=center][font=&][font=宋体]表1 流动相洗脱程序[/font][/font][/align][align=center][font=&][font=宋体][img=,559,298]https://ng1.17img.cn/bbsfiles/images/2023/08/202308151105132742_2164_3963412_3.jpg!w559x298.jpg[/img][/font][/font][/align][align=left][font='Times New Roman','serif']3 [/font][font=宋体]标准品配制：称取一定量的松脂酸，用乙腈[/font][font='Times New Roman','serif']:0.1%[/font][font=宋体]磷酸（[/font][font='Times New Roman','serif']V/V=70:30[/font][font=宋体]）溶解，定容，得到浓度为[/font][font='Times New Roman','serif']200 μg/mL[/font][font=宋体]，待测。[/font][/align][font=宋体][/font][align=center][img=,534,242]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150902130177_1955_3963412_3.jpg!w534x242.jpg[/img]图2 标准品色谱图[/align][align=left][font='Times New Roman','serif']4[/font][font=宋体]样品制备：[/font][/align][align=left][font='Times New Roman','serif']4.1[/font][font=宋体]松香用研钵研碎，称取一定量的样品，用乙腈[/font][font='Times New Roman','serif']:0.1%[/font][font=宋体]磷酸（[/font][font='Times New Roman','serif']V/V=70:30[/font][font=宋体]）超声溶解，定容至[/font][font='Times New Roman','serif']50 mL[/font][font=宋体]，然后过滤待测。[/font][/align][align=center][img=,532,236]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150904090783_7851_3963412_3.jpg!w532x236.jpg[/img][/align][align=center]图3 松香样1色谱图[/align][align=center][/align][align=center][img=,498,227]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150904412965_7172_3963412_3.jpg!w498x227.jpg[/img][/align][align=center]图4 松香样2色谱图[/align][align=left]4.2 称取一定量的液体原药，用乙腈:0.1%磷酸（V/V=70:30）溶解，定容至50mL, 过0.45μm滤膜，待测。[/align][align=center][img=,560,254]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150908303829_927_3963412_3.jpg!w560x254.jpg[/img]图5 原药1色谱图[/align][align=center][img=,513,235]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150908401428_7495_3963412_3.jpg!w513x235.jpg[/img]图6 原药2色谱图[img=,690,516]https://ng1.17img.cn/bbsfiles/images/2023/08/202308150914267479_9450_3963412_3.jpg!w690x516.jpg[/img]图7 松香（1和2）样品图[/align][align=left]结论：从松香质地能看出来松香2 质地要优于松香1，松香1中松香酸含量44.3%，松香2中松香酸含量88.5%，原药1含量12.5%，原药2中含量42.1%。后来联系客户说松香1是湿地松得到的，松香2是马尾松得到的。不同植物得到的松香差异比较明显。[/align][font='Times New Roman','serif'][/font][align=left][font=宋体][/font][/align][align=center][/align][align=left][/align][align=left][/align]

松脂化学组成分析，用气质做的，峰的分离效果已经优化好，现在定性出现新的问题，45min之后的出峰谱库搜索很多重复，保留时间53.6393、53.7428、53.9045、53.9951、54.0857、54.228、55.4117、55.7093、55.9098、55.9616、56.1944、56.4726、56.589、57.1001、57.9669出来的15个峰谱库搜索均为1-Phenanthrenecarboxylic acid, 1,2,3,4,4a,9,10,10a-octahydro-1,4a-dimethyl-7-(1-methylethyl)-, methyl ester, -。按照理论，应该是各种不同的松香酸（同分异构体）。我们谱库是NIST05，是否需要再安装什么专业库才能解决问题？http://ng1.17img.cn/bbsfiles/images/2011/08/201108290930_312669_1912751_3.jpg

10，抽取5个版友）；中奖名单：吕梁山（注册ID：shih20j07）千层峰（注册ID：jxyan）夏天的雪（注册ID：bingwang228）vm88（注册ID：v2826867）捌道巴拉巴巴巴（注册ID：v3082413）http://ng1.17img.cn/bbsfiles/images/2017/03/201703201518_01_1610895_3.jpghttp://ng1.17img.cn/bbsfiles/images/2017/03/201703201518_02_1610895_3.jpg【注意事项】同样的答案，每人只能发一次PS：该贴浏览权限为“回贴仅作者和自己可见”，回复的版友仅能看到版主的题目及自己的回答内容，无法看到其他版友的回复内容。下午3点之后解除，即可看到正确答案、获奖情况及所有版友的回复内容。=======================================================================妇科调经片中阿魏酸的测定(2010药典)方法：HPLC基质：药品应用编号：103057化合物：阿魏酸固定相：Platisil ODS色谱柱/前处理小柱：Platisil ODS 5u 250 x 4.6 mm样品前处理：对照溶液：取阿魏酸对照品适量，用甲醇制成每1 mL含5 μg的溶液。 供试品溶液：取本品10片，除去包衣，精密称定，至具塞锥形瓶中，精密加入甲醇15 mL，称定重量，超声60 min，放冷，再称定重量，用甲醇补足减失的重量，摇匀，滤过，取续滤液，即得。色谱条件：色谱柱：Platisil C18，250×4.6 mm，5 μm (Cat#：99503) 流动相：甲醇：0.1%磷酸溶液=30:70 流速：1.0 mL/min 柱温：30 ℃ 检测器：UV 320 nm 进样量：10 μL文章出处：天津应用实验室关键字：妇科调经片、阿魏酸、铂金、2010药典、含量测定、HPLC谱图：http://www.dikma.com.cn/Public/Uploads/images/11(42).PNGhttp://www.dikma.com.cn/Public/Uploads/images/22(23).PNG图例：1-阿魏酸

问题：妇科调经片中阿魏酸的检测：用到了迪马的哪几款色谱柱，可以满足药典的要求？答案：Diamonsil C18(2)，Diamonsil C18，Platisil ODS三款液相色谱柱【活动奖励】幸运奖（2钻石币）莫名其妙（ID：moyueqiu）大川之子,纵横四海（ID：chuangu120）langyabeilei（注册ID：langyabeilei）http://ng1.17img.cn/bbsfiles/images/2015/11/201511301521_575614_1610895_3.jpghttp://ng1.17img.cn/bbsfiles/images/2015/11/201511301521_575615_1610895_3.jpg积分奖励：所有回答正确的版友奖励10个积分（幸运奖获得者除外）。【注意事项】同样的答案，每人只能发一次PS：该贴浏览权限为“回贴仅作者和自己可见”，回复的版友仅能看到版主的题目及自己的回答内容，无法看到其他版友的回复内容。下午3点之后解除，即可看到正确答案、获奖情况及所有版友的回复内容。妇科调经片中阿魏酸的检测样品制备 制备方法1. 对照品：取阿魏酸对照品适量，精密称定，置棕色量瓶中，加50%乙醇制成每1 mL含5 μg的溶液，即得。2. 供试品：取本品20片，除去包衣，精密称定，研细，取约0.5 g，精密称定，置具塞锥形瓶中，精密加入50%乙醇25 mL，密塞，称定重量，超声处理（功率320 W，频率40 kHz) 30分钟，放冷，再称定重量，用50%乙醇补足减失的重量，摇匀，滤过，取续滤液，即得。分析条件 色谱柱Diamonsil C18(2) 250 x 4.6 mm，5 μm (Cat#：99603)流动相乙腈：0.3%磷酸溶液=18.5：81.5流速1.0 mL/min柱温30 ℃检测器UV 320 nm进样量10 μL 色谱图对照品http://ng1.17img.cn/bbsfiles/images/2015/11/201511300959_575517_1987954_3.png 峰号 保留时间 min 峰面积 μV*s 峰高 μV 理论塔板数* N USP拖尾因子 分离度 1 14.287 345988 21222 17663.367 1.014 -- *药典要求理论板数按阿魏酸峰计算应不低于3000供试品http://ng1.17img.cn/bbsfiles/images/2015/11/201511301000_575518_1987954_3.png 峰号 保留时间 min 峰面积 μV*s 峰高 μV 理论塔板数* N USP拖尾因子 分离度 1 14.197 295224 17993 17421.218 1.008 -- *药典要求理论板数按阿魏酸峰计算应不低于3000本品种同时使用了Diamonsil C18、Platisil ODS两款色谱柱，在药典规定条件下进行阿魏酸的检测，均满足药典要求。

高效液相可同时测定植酸、黄酮和阿魏酸吗？检测波长该如何选择？流动相呢？阿魏酸：有顺式和反式两种，顺式为黄色油状物，反式为正方形结晶或纤维结晶，溶点为174℃，溶于热水，乙醇和乙酸乙酯，稍溶于乙醚，难溶于苯和石油醚。[img]http://ng1.17img.cn/bbsfiles/images/2009/12/200912231143_191530_1638724_3.jpg[/img]黄酮：天然黄酮类化合物多以苷类形式存在 ，并且由于糖的种类、数量、联接位置及联接方式不同可以组成各种各样黄酮苷类。黄酮苷一般易溶于水、乙醇、甲醇等极性强的溶剂中；但难溶于或不溶于苯、氯仿等有机溶剂中。糖链越长则水溶度越大。黄酮类化合物因分子中多具有酚羟基，故显酸性。酸性强弱因酚羟基数目、位置而异。[img]http://ng1.17img.cn/bbsfiles/images/2009/12/200912231143_191531_1638724_3.jpg[/img]植酸：淡黄色浆状液体，易溶于水、乙醇、丙酮，不溶于无水乙醚、苯、已烷、氯仿。[img]http://ng1.17img.cn/bbsfiles/images/2009/12/200912231144_191532_1638724_3.jpg[/img]

【作者】 魏智勇； 王俊华； 边景； 毕丽萍； 刘芳； 周晶； 张庆伟；【机构】 天津传染病医院天津市肝病研究所； 天津医科大学；【摘要】 目的:建立同时测定抗纤丸中芍药苷、阿魏酸、黄芩苷3种有效成分的含量方法。方法:Diamonsil C18色谱柱,流动相甲醇-1%磷酸,梯度洗脱;二极管阵列检测器(DAD);检测波长分别为芍药苷230nm,阿魏酸316nm,黄芩苷280nm,柱温35℃。结果:在3个波长下同时测定3种化合物的含量:芍药苷、阿魏酸、黄芩苷的线性范围分别为0.20~0.60μg,0.025~0.075μg,1.25~3.75μg;平均加样回收率分别为100.87%,100.31%,101.05%;RSD分别为1.03%,0.71%,1.88%。结论:该方法灵敏准确、重复性好,可用于本制剂的质量控制。 【谱图】 http://ng1.17img.cn/bbsfiles/images/2012/08/201208142023_383857_1609970_3.jpg