水質(zhì)19種藻毒素的測(cè)定 液相色譜-串聯(lián)質(zhì)譜法

（資料性附錄）方法檢出限和測(cè)定下限表A.1給出了19種藻毒素的方法檢出限和測(cè)定下限。表A.1方法檢出限和測(cè)定下限序號(hào)目標(biāo)化合物英文名稱CASNo.化學(xué)式方法檢出限（ng/L）測(cè)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環(huán)亞胺毒素（GYM）Gymnodimine173792-58-0C32H45NO40.83.25蛤毒素-2（PTX2）Pectenotoxin-297564-91-5C47H70O1428613-去甲螺旋內(nèi)酯C（SPX1）13-desmethylspirolideC334974-07-1C42H61NO7287大田軟海綿酸（OA）Okadaicacid78111-17-8C44H68O13288鰭藻毒素1（DTX1）Dinophysistonxin-181720-10-7C45H70O13289鰭藻毒素2（DTX2）Dinophysistonxin-2139933-46-3C44H68O131410節(jié)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（資料性附錄）標(biāo)準(zhǔn)使用液濃度表B.1給出了19種藻毒素標(biāo)準(zhǔn)使用液的濃度。表B.119種藻毒素標(biāo)準(zhǔn)使用液的濃度序號(hào)目標(biāo)化合物溶劑標(biāo)準(zhǔn)使用液濃度（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（資料性附錄）目標(biāo)化合物的測(cè)定參考參數(shù)表C.1給出了目標(biāo)化合物的保留時(shí)間及多離子反應(yīng)監(jiān)測(cè)條件等測(cè)定參考參數(shù)。表C.1目標(biāo)化合物的保留時(shí)間、多離子反應(yīng)監(jiān)測(cè)條件等測(cè)定參考參數(shù)目標(biāo)化合物保留時(shí)間（min）采集模式母離子（m/z）定量子離子定性子離子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（資料性附錄）方法的精密度和正確度表D.1～D.2給出了方法的精密度和正確度匯總數(shù)據(jù)。表D.1精密度匯總表序號(hào)目標(biāo)化合物加標(biāo)濃度（ng/L）實(shí)驗(yàn)室內(nèi)相對(duì)標(biāo)準(zhǔn)偏差（%）實(shí)驗(yàn)室間相對(duì)標(biāo)準(zhǔn)偏差（%）重復(fù)性限（ng/L）再現(xiàn)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正確度匯總表序號(hào)目標(biāo)化合物加標(biāo)濃度（ng/L）地表水海水回收率范圍（%）（%）回收率范圍（%）（%）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