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(资料性附录)方法检出限和测定下限表A.1给出了19种藻毒素的方法检出限和测定下限。表A.1方法检出限和测定下限序号目标化合物英文名称CASNo.化学式方法检出限(ng/L)测定下限(ng/L)1原多甲酸毒素1(AZA1)Azaspiracid-1214899-21-5C47H71NO12182原多甲酸毒素2(AZA2)Azaspiracid-2265996-92-7C48H73NO12283原多甲酸毒素3(AZA3)Azaspiracid-3265996-93-8C46H69NO12184环亚胺毒素(GYM)Gymnodimine173792-58-0C32H45NO40.83.25蛤毒素-2(PTX2)Pectenotoxin-297564-91-5C47H70O1428613-去甲螺旋内酯C(SPX1)13-desmethylspirolideC334974-07-1C42H61NO7287大田软海绵酸(OA)Okadaicacid78111-17-8C44H68O13288鳍藻毒素1(DTX1)Dinophysistonxin-181720-10-7C45H70O13289鳍藻毒素2(DTX2)Dinophysistonxin-2139933-46-3C44H68O131410节球藻素(NOD)Nodularin118399-22-7C41H60N8O102811微囊藻毒素-RR(MC-RR)Microcystin-RR111755-37-4C49H75N13O122812微囊藻毒素-YR(MC-YR)Microcystin-YR101064-48-6C52H72N10O1331213微囊藻毒素-HtyR(MC-HtyR)Microcystin-HtyR478001-08-0C53H74N10O1331214微囊藻毒素-LR(MC-LR)Microcystin-LR101043-37-2C49H74N10O122815微囊藻毒素-WR(MC-WR)Microcystin-WR138234-58-9C54H73N11O1231216微囊藻毒素-LA(MC-LA)Microcystin-LA96180-79-9C46H67N7O122817微囊藻毒素-LY(MC-LY)Microcystin-LY123304-10-9C52H71N7O132818微囊藻毒素-LW(MC-LW)Microcystin-LW157622-02-1C54H72N8O1231219微囊藻毒素-LF(MC-LF)Microcystin-LF154037-70-4C52H71N7O1228(资料性附录)标准使用液浓度表B.1给出了19种藻毒素标准使用液的浓度。表B.119种藻毒素标准使用液的浓度序号目标化合物溶剂标准使用液浓度(μg/L)1AZA1甲醇2602AZA2甲醇2443AZA3甲醇2364GYM甲醇1255PTX2甲醇2206SPX1甲醇2517OA甲醇4208DTX1甲醇3909DTX2甲醇19010NOD甲醇50011MC-RR甲醇50012MC-YR甲醇50013MC-HtyR甲醇50014MC-LR甲醇50015MC-WR甲醇50016MC-LA甲醇50017MC-LY甲醇50018MC-LW甲醇50019MC-LF甲醇500(资料性附录)目标化合物的测定参考参数表C.1给出了目标化合物的保留时间及多离子反应监测条件等测定参考参数。表C.1目标化合物的保留时间、多离子反应监测条件等测定参考参数目标化合物保留时间(min)采集模式母离子(m/z)定量子离子定性子离子m/z碰撞能(eV)m/z碰撞能(eV)MC-RR4.632ESI+519.8135.236105.049NOD4.684ESI+825.5135.260227.055GYM4.826ESI+508.4490.330392.340MC-YR5.086ESI+523.4135.230911.530MC-HtyR5.087ESI+1059.2135.155107.160MC-LR5.096ESI+995.4135.265213.164MC-WR5.461ESI+1068.5135.265213.164SPX15.480ESI+692.5164.140444.240MC-LA6.326ESI+910.4135.260213.150MC-LY6.947ESI+1002.4135.255127.040MC-LW8.637ESI+1025.4135.260213.160MC-LF8.752ESI+986.4135.260478.140AZA310.111ESI+828.5810.535792.540PTX210.164ESI+876.6823.035212.740AZA110.465ESI+842.6824.635806.640AZA210.706ESI+856.5838.545820.550OA4.908ESI-803.5255.050113.050DTX25.118ESI-803.5255.250113.050DTX15.648ESI-817.5255.250113.040(资料性附录)方法的精密度和正确度表D.1~D.2给出了方法的精密度和正确度汇总数据。表D.1精密度汇总表序号目标化合物加标浓度(ng/L)实验室内相对标准偏差(%)实验室间相对标准偏差(%)重复性限(ng/L)再现性限(ng/L)地表水海水地表水海水地表水海水地表水海水1AZA113.03.5~113.0~3.24.14.8218.6218.626.01.7~3.91.4~5.86.85.67.5127.81252.00.6~5.81.2~2.96.37.69.55.611.8112AZA212.22.6~114.8~115.12.421252125.24.41.0~5.01.9~9.19.35.71117111748.80.7~1.21.8~3.46.64.72.67.88.09.03AZA311.83.9~127.4~145.94.22132213223.61.0~4.61.2~3.66.44.59.67.69.67.647.21.0~2.21.4~4.57.62.24.68.39.58.34GYM6.255.9~7.47.3~139.5191929192912.55.1~111.6~7.715142317231725.03.0~6.31.5~7.5199.415.1419145PTX211.04.6~6.82.1~186.6131736173622.03.5~6.92.8~4.31515149.9141244.01.2~3.92.2~9.49.66.78.61713176SPX112.56.0~124.9~1214172524252425.11.8~7.53.3~8.1144.51417171750.14.1~8.24.9~7.51918191830277OA21.02.3~7.62.8~1220151623182342.00.6~9.71.4~3.02.013166.3161584.01.6~4.70.6~6.86.4159.01316358DTX119.51.7~6.53.3~9.7187.61518161839.01.6~130.8~5.7195.22412271278.01.9~5.90.6~8.9127.8111824249DTX29.502.4~111.6~9.79.5202217221719.01.2~4.41.7~3.42.8118.87.58.88.838.01.4~6.31.2~5.3127.3159.4181210NOD20.01.8~122.6~6.713142216221650.00.9~4.61.5~8.113169.01814.7251002.3~5.92.9~5.67.4161212204111MC-RR20.04.3~5.27.6~12165.71427142750.04.1~8.72.7~8.08.611181618171004.1~7.42.7~5.9196.91614381812MC-YR20.03.7~5.83.5~1114.62.61520152050.04.3~9.33.8~114.74.6232323231005.4~5.91.3~6.55.82.31611211213MC-HtyR20.02.6~8.93.2~13189.41825192550.06.1~113.0~6.6166.6261531151003.1~6.63.5~7.38.14.41417241814MC-LR20.04.8~133.3~119.25.62321232150.03.3~8.74.8~9.15.33.8191919191001.6~5.14.3~7.44.4111216163115MC-WR20.03.1~9.67.7~122.12.41827182750.02.3~7.62.6~5.30.42.3171217121005.2~7.01.2~4.57.14.91811201216MC-LA20.02.9~124.8~127.79.22122212250.03.9~7.75.1~126.70.5162318231001.3~4.81.6~4.63.54.51111141717MC-LY20.02.7~8.66.1~9.84.2132022202250.05.6~6.46.4~9.31716182324271001.7~2.91.2~9.113206.716274918MC-LW20.04.1~9.07.1~133.32.81828182850.02.3~6.13.2~7.13.13.4121512151002.2~7.14.5~6.42.82.11616161619MC-LF20.04.0~9.54.7~6.620181916191750.04.4~6.32.1~4.31814159.223181003.9~4.22.3~8.2199.112154627表D.2正确度汇总表序号目标化合物加标浓度(ng/L)地表水海水回收率范围(%)(%)回收率范围(%)(%)1AZA11363.8~68.767.0±5.566.7~73.070.5±6.72671.3~81.676.6±10.473.5~82.077.2±8.75281.0~91.986.3±5.576.0~88.482.4±6.72AZA212.264.1~71.167.8±7.069.5~72.571.5±3.424.472.5~85.977.7±14.473.2~81.977.4±8.848.880.0~91.085.0±7.080.2~87.784.6±3.43AZA311.863.1~71.066.9±8.065.6~71.268.8±5.823.672.5~81.475.9±9.772.9~79.876.4±6.947.280.4~92.785.4±8.080.2~83.882.1±5.84GYM6.2559.3~70.763.8±12.157.0~82.569.7±25.512.565.5~87.278.3±22.765.4~85.375.6±19.92582.6~11594.6±12.168.9~81.677.2±25.55PTX21151.9~58.654.5±7.276.0~96.484.2±21.62253.6~71.762.2±18.280.1~10388.0±25.94478.0~93.784.6±7.278.4~89.684.7±21.66SPX112.567.5~88.379.7±21.760.0~83.772.8±23.925.186.6~11499.9±27.780.9~88.385.1±7.650.174.6~10993.0±21.772.1~10388.3±23.97OA2175.3~11090.4±36.080.0~10792.3±27.64286.1~89.287.1±3.684.9~10693.3±23.08484.7~96.191.2±36.086.6~11296.4±27.68DTX119.560.7~86.574.2±25.975.1~87.381.8±12.43962.1~90.079.2±29.985.8~94.489.1±9.37875.6~95.185.7±25.991.2~10697.2±12.49DTX29.572.5~87.581.0±15.474.5~11091.5±35.31985.5~90.287.5±4.987.0~10794.9±20.83886.9~10996.1±15.490.6~10598.2±35.310NOD2064.2~81.471.0±18.272.1~93.881.9±22.05062.8~79.870.1±17.576.8~10186.1±26.310071.8~83.377.8±18.281.9~10690.0±22.011MC-RR2051.0~68.558.8±17.952.7~58.254.7±6.25054.7~64.759.0±10.252.3~63.056.2±11.910051.7~76.164.7±17.961.8~70.367.1±6.212MC-YR2079.6~10287.0±25.577.4~81.579.2±4.25086.1~93.888.9±8.474.9~81.279.1±7.210087.9~98.793.6±25.586.1~90.288.2±4.213MC-HtyR2067.6~97.183.6±29.870.3~83.375.1±14.25075.8~10388.6±27.372.5~81.976.2±10.110081.5~95.988.7±29.880.7~87.283.0±14.214MC-LR2075.9~91.283.4±15.370.3~77.572.8±8.150

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